BP 306 P For Publication Final

Including
Innovative
A Practical Book of Practical’s
Physical Pharmaceutics - I
(Strictly as per syllabus prescribed for Bachelor of Pharmacy)
Semester-III by Pharmacy Council of India, New Delhi
B.Pharm. IInd Year
IIIrd Semester
Mr. Nirmal Morya Ms. Komal Verma

M.Pharma (Gold Medalist), DOAP M.Pharm. (Pharmacology)
Assistant Professor Assistant Professor
Pranveer Singh Institute Babu Banarasi Das University
Technology (Pharmacy), Lucknow
Kanpur
Dr. Pranay Wal Mr. Shashi Pratap Singh

M.Pharm., Ph.D. M.Pharma (Pharmacology) PhD.(P)
Dean, Professor Assistant Professor
Pranveer Singh Institute of Pranveer Singh Institute
Technology (Pharmacy), Technology (Pharmacy),
Kanpur Kanpur
Preface
This book's primary goal is to introduce the basic ideas of Physical Pharmaceutics - I practical’s
so that readers can enhance their skills in physical pharmaceutics. It is related to physical
characteristics of pharmaceutical compound in the form of pure drug or dosage form. The main
focus is on conceptual significance and easy understanding, as well as easy observational and
calculation process. To fully comprehend the subject, conceptual ideas underlying practical
elements are taught. To promote students, additional safety measures for laboratory work and
viva-voce questions are also provided. To improve critical thinking skills, these questions range
from the extremely simple to the moderately tough.
There are several learning goals in this book's writing. The student should be able to understand
the fundamental ideas of Physical Pharmaceutics-I after reading this book, including how to
handle chemical, determine physical properties, grasp the function of each process, and lastly
analyses physical properties.
The primary audience for this text is pharmacy undergraduate students. Graduate students
studying pharmaceutics and other biomedical disciplines, however, might also find it helpful. We
anticipate that this book will be especially beneficial for students who have previously found it
challenging and unattainable to master the concepts and abilities required for Physical
Pharmaceutics - I.
We are grateful to TDC publication team for publishing a book on schedule and with high
quality. Above all, we give thanks to the Almighty for bringing us to the point where we
could work to realize a deeply held dream.
Author
Nirmal Morya
Komal Verma
Dr. Pranay Wal
Shashi Pratap Singh

Acknowledgement
We are extremely thankful to Dr. A.K. Rai (Director- Pranveer Singh Institute of Technology-
Pharmacy) and Dr. Ankita Wal (Head of Department- Pranveer Singh Institute of Technology-
Pharmacy) or their guidance suggestion & appreciation.
TDC Publication and their employees are acknowledged for their active support in bringing out
the book at an appropriate time.
Nirmal Morya
Komal Verma
Dr. Pranay Wal
Shashi Pratap Singh

About the Authors
NIRMAL MORYA is a faculty at Pranveer Singh Institute of technology, Bhauti Kanpur Nagar,
U.P., with 3 years of teaching experience. He has completed his B.Pharm from KIET School of
Pharmacy (KIET Group of Institution) Ghaziabad U.P. and M.Pharm in Pharmaceutics (Gold
Medalist) from Babasaheb Bhimrao Ambedkar University (A Central University) Lucknow. He
has completed Diploma in Office Automation and Publishing (DOAP) and completed a
certificate course in course on computer concepts (CCC). He has qualified national level
examination in Pharmacy (Graduate Pharmacy Aptitude Test – GPAT) in 2018 & 2021. He is
attended 3 Days Entrepreneurship Awareness Camp organized by TBI-KIET Ghaziabad. He is
the registered pharmacist under Delhi Pharmacy Council New Delhi. He is the life member of
registered pharmacist welfare trust Govt. NCT Delhi. He has 1 publication and 2 textbook to his
credit. He is attended many conferences and Faculty Development Programs (FDPs).
KOMAL VERMA is a faculty at School of Pharmacy, Babu Banarasi Das University Lucknow
U.P., with 3 years of teaching experience. She has completed her B.Pharm from Kanpur Institute
of Technology Kanpur. And M.Pharm (Pharmacology) from Babasaheb Bhimrao Ambedkar
University (A Central University) Lucknow, She has qualified national level examination in
Pharmacy (Graduate Pharmacy Aptitude Test – GPAT) in 2019. She is the registered pharmacist
under Uttar Pradesh Pharmacy Council Lucknow. She has 1 publication and 1 textbook to her
credit. She is attended many conferences and Faculty Development Programs (FDPs).
Dr PRANAY WAL is working as Professor & Dean Pharmacy in PSIT Kanpur. He has
published more than 50 national and international papers in reputed journals (SCI/ Scopus). Has
got grants from various government agencies worth rupees more than 80 lakhs (AICTE, DST,
UPCST, ICMR, CSIR, NSTEDB). Has filled more than 30 patents till date and out of which 15
Patents are Granted. He is involved in medical device development with scientists from IIT
Kanpur & NIPER. Constantly involved in guiding students for GRE, TOFEL and other life
science options after intermediate and encouraging young students to develop themselves for the
healthcare sector of India. Have also associated with some international universities abroad.
Working as Nodal Officer for NIRF and for Accreditation of NAAC & NBA. An active Member
of International Pharmaceutical federation (FIP) and Young pharmacist Association group,
Netherland, Participated in FIP BASEL, Switzerland. Serving as a Reviewer for: Journal of
Pharmacy Practice, International journal of Pharmaceutical science and Biotechnology, African
Journal of Pharmacy and Pharmacology, Journal of Pharmaceutical science and Research, Serial
Publications etc. Constantly writing chapters in books for Elsevier, and has published eight
books till date. He has organized more than 25 National & International Events, Conferences,
and workshops, FDPs, STTP etc. as Convener or Organizing Secretary. Life Member of RED
CROSS Society and participated and conducted AIDS Eradication and Polio awareness
programs in various districts of India. He has an excellent track record in academics (Qualified
GATE two times) He has presented his research work in International pharmaceutical federation
(FIP-08) in Basel, Switzerland. (Funded By CSIR). Have completed 6 Months Course from
Manipal University on Biostatistics & Research Methodology, also completed 3 months course
from EDI Ahmedabad, on educators of mentors, apart from this completed Valuation of Startups
MDP from IIM Lucknow, boot camp on prototype development from IIT Kanpur and CCAMP
Bangalore. Also completed the IPR Course of WIPO Geneva and PDCR for Clinical Trials
SHASHI PRATAP SINGH is a faculty at Pranveer Singh Institute of technology, Bhauti

Kanpur Nagar, U.P., with 5 years of teaching experience. He has pursuing Ph.D. in
Pharmaceutical Sciences from NIMS University Jaipur, Rajasthan. He has completed his
B.Pharm and M.Pharm (Pharmacology) from Pranveer Singh Institute of technology, Bhauti
Kanpur. He is a life member of Association of Pharmaceutical Teacher of India (APTI). He has
20 publication and 4 text books to his credit attended many National and International
conferences, Seminars, FDP and Workshops. Have completed 12 weeks “Online Refresher
Course in Pharmacy for Higher Education” with a "A" Grade in the proctored examination from
Indian Institute of Technology (BHU) Varanasi, also completed NPTEL course Health Research
Fundamentals (8 Weeks) on the SWAYAM platform, completed online course “Academic
writing” on the SWAYAM platform with 4 credit score and completed online course “Industrial
Pharmacy” on the SWAYAM platform.
Syllabus
1. Determination the solubility of drug at room temperature.
2. Determination of pKa value by Half Neutralization/Henderson Hesselbalch

equation.
3. Determination of Partition coefficient of benzoic acid in benzene and water.
4. Determination of Partition coefficient of Iodine in CCl4 and water.
5. Determination of % composition of NaCl in a solution using phenol-water

system by CST method.
6. Determination of surface tension of given liquids by drop count and drop weight
method.
7. Determination of HLB number of a surfactant by saponification method.
8. Determination of Freundlich and Langmuir constants using activated char coal.
9. Determination of critical micellar concentration of surfactants.
10. Determination of stability constant and donor acceptor ratio of PABA-Caffeine

complex by solubility method.
11. Determination of stability constant and donor acceptor ratio of Cupric Glycine
complex by pH titration method.
Content
LIST OF EXPERIMENT
Sr. No. Title Page No.
1 To determine the solubility of given sample at different temperature.
2 To determine pKa value of given sample by Half Neutralization/
Henderson Hesselbalch equation
3 To determine partition coefficient of benzoic acid in benzene and
water.
4 To determine partition coefficient of Iodine in CCl4 and water
5 To determine unknown % composition of NaCl in a solution using
phenol-water system by CST method
6 To determine surface tension of given liquids by drop count and drop
weight method
7 To determine HLB number of a given surfactant by saponification
method
8 To determine specific surface area and monolayer capacity (Freundlich
and Langmuir isotherm) using activated char coal
9 To determine critical micellar concentration (CMC) of given surfactant
10 To determine stability constant and donor acceptor ratio of PABA-
Caffeine complex by solubility method
11 To determine stability constant and donor acceptor ratio of Cupric-
Glycine complex by pH titration method.
12 To determine viscosity of given liquid by using Ostwald viscometer.

13 To study flow properties of powder and effect of lubricant on flow
properties
Experiment No. 01
Aim: To determine the solubility of given sample at different temperature.
Requirements: Salts (KCI, NaCl), Distilled water, t hermometer, Porcelain dishes or watch glasses,
Beaker, Pipette (10 ml), Hot plate
Theory: Solubility is defined in quantitative terms as the concentration of solute in a saturated
solution at a certain temperature. Qualitatively it is defined as a spontaneous interaction of two or
more substances to form a homogeneous molecular dispersion.
Quantitatively, solubility is expressed in molality, molarity, and percentage (w/v or w/w). A
saturated solution is defined as the one in which the solute is in equilibrium with the solid phase
(solute) at a certain temperature. A solution may sometimes contain more amount of solute than
in saturated one; such a solution is known as "Super saturated solution".
The solubility of the solid depends on temperature, melting point of the solid and molar heat of
fusion.
A curve drawn between solubility and temperature is termed as solubility curve. It shows the
effect temperature on the solubility of a substance. The solubility curves of substance like
calcium acetate, calcium chromate show decrease in solubility with increase of temperature
while there are others like those of sodium nitrate and lead nitrate, which show an increase of
solubility with temperature. The solubility curve of sodium chloride shows very little rise with
increase of temperature.
There are two types of solubility curves:
1. Continuous solubility curves: regular changes in solubility with temperature.
Example: Calcium salts of fatty acids, lead nitrate.
2. Discontinuous solubility curves: irregular changes in solubility with temperature.
Example: Sodium Sulphate, Ferric chloride.
Fig.1 Solubility curve of different salts
In this study the effect of temperature on NaCl solubility will be carried out.
Procedure:
1. Clean all glassware’s using detergent solution.

2. Wash two to three times using purified water
3. Take 50 ml of distilled water in a beaker (100 ml).
4. Add some amount of salt like potassium chloride or sodium chloride in distilled water
and stir using glass rod or by an electric motor driven shaker.
5. Increase the temperature to 85°C with continuous stirring.
6. Maintain this temperature for few minutes and then cool down the solution.
7. Take sample at 80°C using a pipette with a piece of filter paper, tie at the tip of the
pipette.
8. Remove the piece of filter paper from the tip of pipette and transfer 10 ml of this solution
in weighed porcelain dish or watch glass.
9. Allow the temperature to fall down slowly to 70°, 60°, 40°, 30°C and then to room
temperature.
10. At each temperature take sample of the solution and repeat the step 7 and step 8.
11. Evaporate the solution of each porcelain dish or watch glass using direct heat or on the
water bath or put in the oven.
12. Dry the solution till constant weight.
13. Take weight of the dish using balance.
14. Record all the parameter in the form of table or in proper way so that it was easy to
understand the concept of solubility,
Observation
Table1: Observation table for solubility determination
Sr Temp Weight of Weight of Weight of Weight of Weight of

No (oC) empty empty dish + residue Solvent
dish dish + residue (W3 – W1) (W2 – W3) Solubility in
(W1) solution (W3) gm/100 gm
(W2)
Gm
1 80
2 70
3 60
4 40
5 30
6 RT
Calculation:
Solubility of NaCl in solvent (DW) at different temperature (°C) is calculated by the following
formula in g/100g
Solubility of NaCl at (…oC) = (W3 – W1 / W2 –W3) * 100
Result:
i. Solubility of NaCl at different temperature was determined.

Table 2: solubility of salt
Sr No Temp Solubility in gm/100 gm
(oC)
1 80
2 70
3 60
4 40
5 30
6 RT
ii. Graph was plotted solubility per 100 gm (Y-axis) vs temperature (X-axis) and
found ……………………….. (continuous/discontinuous) solubility curve.
Fig.2 solubility vs Temperature curve
VIVA-VOCE QUESTIONS AND ANSWERS

1. Define solubility.
In chemistry, solubility is the ability of a substance, the solute, to form a solution with
another substance, the solvent. Insolubility is the opposite property, the inability of the solute
to form such a solution.
2. Define solvent.
A solvent is a substance that dissolves a solute, resulting in a solution. A solvent is usually a
liquid but can also be a solid, a gas, or a supercritical fluid.
3. Define solute.
A substance that is dissolved in a solution is called a solute.
4. Effect of temperature on solubility.

In general, solids become more soluble as the temperature increases. This is why sugar
dissolves better in hot water than in cold water. The table shows three examples of the
solubility (g of solute per 100 g water) of substances at different temperatures
5. What is the meaning of solubility curve?

A curve drawn between solubility and temperature is termed as solubility curve. It shows the
effect temperature on the solubility of a substance. The solubility curves of substance like
calcium acetate, calcium chromate show decrease in solubility with increase of temperature
while there are others like those of sodium nitrate and lead nitrate, which show an increase of
solubility with temperature. The solubility curve of sodium chloride shows very little rise
with increase of temperature.
There are two types of solubility curves:
1. Continuous solubility curves: regular changes in solubility with temperature.
Example: Calcium salts of fatty acids, lead nitrate.
2. Discontinuous solubility curves: irregular changes in solubility with temperature.
Example: Sodium Sulphate, Ferric chloride.
Experiment No. 02
Aim: To determine pKa value of the given sample (acetic acid) by Henderson Hesselbalch
equation (pH meter).
Requirement: beaker, volumetric flask, glass rod, pH meter, acetic acid, distilled water.
Theory: pH of the solution is the negative logarithm to the base 10 of H + ion concentration in
solution. Therefore, pH = -log [H+] = -log C H. The solution of pH 7 is called neutral solution. A
solution of pH between 0 and 7 is considered acidic and that between 7 to 14 is considered to be
alkaline solution. pH of a solution can be determined by using Hydrogen ion indicator. For
example, Methyl red shows its full alkaline colour, yellow, at pH of about 6 and its full acid
colour, red; at about pH 4.
Determination of pH using pH meter is quite easy and accurate when compared to other method.
pH can be calculated by using Henderson Hesselbalch equation which is given as:
(Conjugate base)
pH= pKa+log For weak acid
( Acid )
Fig.3 Relationship between Ka and pKa

Consider that the weak acid, acetic acid has undergone dissociation and not a complete
dissociation.
CH3COOH + H2O CH3COO- + H3O+
Procedure
Method-1
1. Calibrate pH meter using standard buffer tablet.

2. Take 0.05ml of acetic acid and make up volume up to 100ml with DW.
3. Transfer this to a beaker and measure the pH.
4. Calculate pKa using the equation.
Calculation
Density of Acetic acid or weight per ml = 1.0495 gm/cm3
Molecular weight of acetic acid = 60.05 gm/mol.
So, 0.05 ml of acetic acid will be equal to = 0.052475 gm
So, 60.05 gm of acetic acid in 1000 ml of water gives = 1M solution
0.052475 gm of Acetic acid in 1000 ml gives = 1 / 60.05 * 0.05247 = 0.00087 moles/L
0.052475 (0.05ml) gm of Acetic acid in 100 ml gives = 0.00087 / 10
= 0.0087 moles/L
Determination of [H+]
pH = -log [H]+
[H] + = 10 - pH
Determination of Ka
Ka = [H+]2 / [HA]- [H]+
[HA]- [H]+ = 0.0087 moles/L
Conversion of Ka to pKa:
pKa= - log Ka
Method-2 (Half neutralization reaction)
Requirements: 0.1N NaOH, phenolphthalein indicator
Procedure:
1. Prepare a solution of 0.0087 mole/L acetic acid (0.05ml of acetic acid in 100ml of DW).
2. 10ml of acetic acid solution titrate with 0.1N NaOH (4gm NaOH in 1000 ml of DW)
using phenolphthalein indicator.
3. At the end point colorless to pink color will appear.
4. Note down volume consumed of NaOH. (Full neutralization). Mark X ml.
5. Again take fresh 10ml solution (0.0087 mole/L) of acetic acid in conical flask.
6. Now add X/2 ml of 0.1N NaOH in the conical flask.
7. Stir well and determine pH of the solution (half neutralization reaction) by using pre-
calibrated pH meter.
8. At half neutralization reaction, pH = pKa.
Calculation
Volume consumed of 0.1NaOH for neutralization of 10 ml Acetic acid (0.0087M) solution = X
Volume consumed of 0.1NaOH for half neutralization of 10 ml Acetic acid (0.0087M) solution =
X/2 ml
After addition of 3ml of 0.1N NaOH in the 10 ml Acetic acid (0.0087M) solution pH was = ….
At half neutralization reaction:
pH = pKa
So pKa = ……
Result: pKa was found to be …………… by half neutralization reaction.
1. Define pH?
A figure expressing the acidity or alkalinity of a solution on a logarithmic scale on which 7 is
neutral, lower values are more acid and higher values more alkaline. The pH is equal to
−log10 c, where c is the hydrogen ion concentration in moles per litre.
2. What is Henderson Hesselbalch equation?

One way to determine the pH of a buffer is by using the Henderson–Hesselbalch equation,
which is pH = pKₐ + log([A⁻]/[HA]). In this equation, [HA] and [A⁻] refer to the
equilibrium concentrations of the conjugate acid–base pair used to create the buffer solution.
3. Define pKa?
pKa is a number that describes the acidity of a particular molecule. It measures the strength
of an acid by how tightly a proton is held by a Bronsted acid. The lower the value of pKa, the
stronger the acid and the greater its ability to donate its protons, Describe the acidity of a
particular molecule
Ka denotes the acid dissociation constant. It measures how completely an acid dissociates in
an aqueous solution. The larger the value of Ka, the stronger the acid as acid largely
dissociates into its ions and has lower pka value. The relationship between pKa and Ka is
described by the following equation: pKa = -log[Ka]
4. What is half neutralization?

In the middle of this gradually curve the half-neutralization occurs. At this point the
concentration of weak acid is equal to the concentration of its conjugate base. Therefore the
pH=pKa. This point is called the half-neutralization because half of the acid has been
neutralized
5. pKa of acetic acid.

pKa of acetic acid is 4.7
Experiment No. 03
Aim - To determine the partition coefficient of Benzoic Acid between benzene (C 6H6) and
distilled water (DW)
Requirements: Benzene, Distilled water, 0.01N NaOH, Separating funnel, conical flask,
Burette, Pipette, Reagent bottles
Theory: Distribution law states that a solute distributes itself between two non-miscible solvents
in contact with each other in such a way that at constant temperature the ratio of its concentration
in the two layers is constant irrespective of its total amount.
If excess of a liquid or solid is added to a mixture of two immiscible liquids, it will distribute
itself between the two phases so that each becomes saturated. If the added substance is in
sufficient to saturate the liquids, it will be distributed between the two layers in a definite
proportion at equilibrium and at constant temperature.
K= Concentration of solute in Organic Phase / Concentration of Solute in Aqueous Phase
= C1 / C2 = Corg/CAq
The equilibrium constant K, is known as Distribution Coefficient or Partition Coefficient.

This is known as Nernst's law or Distribution law.
Benzoic Acid, when distributed between benzene and water, exists mainly as associated
molecule in benzene layer and as an individual molecule i.e. unassociated molecule in aq. Layer
hence the equation is given as:
n √ Concentration of solute∈organic phase n √Corg
K= =
Concentration of solute∈ aqueous phase Caq
n= no of molecule associated with benzene
In this study partition co-efficient will be determined for Benzoic Acid between Benzene and
water.
Preparation of Solutions
a. Preparation of 0.01N Sodium Hydroxide- Dissolve 0.4gm of sodium hydroxide in DW
and dilute of 1000 ml. in volumetric flask.
Procedure
1) Weigh 3 samples (250, 500, 750mg) of benzoic acid in to 3 reagent bottles.
2) Add 50ml of benzene and 50ml of DW in all three bottles.
3) Mark bottles A, B, C, respectively.
4) Place the stopper on each bottle and shake it for 30 min. or shake using wrist action
shaker and rotatory shaker.
5) Variability of the result depends on the shaking hence more and effective shaking is
essential for reproducible results.
6) Now take this mixture in separating funnel and keep aside for about to 30 min.
7) Separate Benzene and aqueous layer in two conical flasks.
8) Intermediate liquid cannot be collected as it contains little of both liquids.
9) Put the label on both conical flasks with the samples taken originally.
10) Pipette out 10 ml of the aqueous layer and transfer in another conical flask and titrate
with 0.01N NaOH Solution.
11) Record the titration value and repeat again for remaining bottle.
12) Similarly, titrate the aqueous layer from other containers.
13) Pipette out 10 ml of benzene layer in a dry and clean conical flask and titrate with 0.01N
NaOH Solution.
14) Similarly, titrate other Benzene solution as previous step.
15) Take all readings carefully
16) Calculate concentration of iodine in both phases i.e. aqueous and organic phase.
Note- Indicator (phenolphthalein) Color Change – Color less to pink.
Fig.4 Titration of Organic Layer
Fig.5 Titration of Aq. Layer

Observation
Table: 3 Titration of Aq. Layer
S. Container Volume Burette Reading Volume of 0.01N NaOH Conc. Of Benzoic Acid
No. V2 (ml) Initial Final consumed in ml (V1) (0.00122 * V1)
1 A 10
2 B 10
3 C 10
Table: 4 Titration of Organic layer (Benzene)

S. Container Volume Burette Reading Volume of 0.01N NaOH Conc. Of Benzoic Acid
No. V2 (ml) Initial Final consumed in ml (V1) (0.00122 * V1)
1 A 10
2 B 10
3 C 10
Calculation
Each ml of 0.01N NaOH = 0.00122 gm of benzoic acid
Table: 5 Determination of partition co efficient of Benzoic Acid
Container Phase Conc. Of benzoic acid √Corganic Partition co

(C) Caqueous efficient
(K)
A Organic
Water
B Organic
Water
C Organic
Water
Result: Partition coefficient value of Benzoic Acid in benzene and water was determined and
found to be …………………………
1. What is the meaning of partition co efficient?

A partition coefficient is the ratio of the concentration of a substance in one medium or phase
(C1) to the concentration in a second phase (C 2) when the two concentrations are at
equilibrium; that is, partition coefficient = (C1/C2)equil.
Benzoic Acid, when distributed between benzene and water, exists mainly as associated
molecule in benzene layer and as an individual molecule i.e. unassociated molecule in aq.
Layer hence the equation is given as:
n √ Concentration of solute∈organic phase n √Corg
K= =
Concentration of solute∈ aqueous phase Caq
n= no of molecule associated with benzene
In this study partition co-efficient will be determined for Benzoic Acid between Benzene and
water.
2. What is the significance of partition coefficient?

Partition coefficients are useful in estimating the distribution of drugs within the body, as it
gives a measure of a solute's hydrophobicity and a proxy for its membrane permeability.
3. What is the unit of partition coefficient?

A partition coefficient essentially has no units (has units of concentration/concentration) and
is typically defined at concentrations far from saturation.
4. What is the use of separating funnel?

A separator funnel is used to separate immiscible liquids. When two immiscible liquids are
placed in a separator funnel, two layers are seen. The denser solvent will be the bottom layer.
Most halogenated solvents are denser than water; most non-halogenated solvents are less
dense than water
5. Does temperature affect partition coefficient?

Partition coefficient generally decreases with temperature. This may be due to increased
solubility of solute in water with temperature rise.
Experiment No. 04
Aim - To determine the partition coefficient of iodine between carbon tetrachloride (CCl 4) and
distilled water (DW)
Requirements: Carbon tetrachloride, Iodine, Distilled water, sodium thio sulphate, KI
Separating funnel, conical flask, Burette, Pipette, Reagent bottles
Theory
Distribution law states that a solute distributes itself between two non-miscible solvents in
contact with each other in such a way that at constant temperature the ratio of its concentration in
the two layers is constant irrespective of its total amount.
If excess of a liquid or solid is added to a mixture of two immiscible liquids, it will distribute
itself between the two phases so that each becomes saturated. If the added substance is in
sufficient to saturate the liquids, it will be distributed between the two layers in a definite
proportion at equilibrium and at constant temperature.
K= Concentration of solute in Organic Phase / Concentration of Solute in Aqueous Phase
= C1 / C2 = Corg/CAq
The equilibrium constant K, is known as Distribution Coefficient or Partition Coefficient.
This is known as Nernst's law or Distribution law.
In this study partition co-efficient will be determined for Iodine between Carbon tetrachloride
and water.
Preparation of Solutions
b. Preparation of 0.1N Sodium Thiosulphate- Dissolve 26gm of sodium thiosulphate
penta hydrate and 0.2 gm of Sodium Carbonate in DW and dilute of 1000 ml. in
volumetric flask.
c. Preparation of 0.005N Sodium thiosulphate- Dissolve 1.3 gm of sodium thiosulphate
penta hydrate and 0.01 gm of Sodium Carbonate in DW and dilute of 1000 ml. in
volumetric flask.
d. Preparation of 10% KI Solution: add 10gm of KI in 100 ml of DW.
e. Preparation of Starch Indicator: dissolve 300mg of Starch in 100ml of distilled water
and heat for proper solubility.
Procedure
1. Prepare a saturated solution of iodine in carbon tetrachloride (stock solution).
2. Take three reagent bottles and clean these bottles by reagent and rinse with it distilled
water.
3. Prepare composition of the solution as given in the table no 6
4. Transfer these solutions in clean and dry reagent bottles and be it as A, B, and C
respectively.
5. Place the stopper on each bottle and shake it for 30 min. or shake using wrist action
shaker and rotatory shaker.
6. Variability of the result depends on the shaking hence more and effective shaking is
essential for reproducible results.
7. Now take this mixture in separating funnel and keep aside for about to 30 min.
8. Separate carbon tetrachloride and aqueous layer in two conical flasks:
9. Intermediate liquid cannot be collected as it contains little of both liquids.
10. Put the label on both conical flasks with the samples taken originally.
11. Pipette out 10 ml of the aqueous layer and transfer in another conical flask and add 10 ml
of 10% KI solution.
12. Add 2 to 3 drops of starch solution and titrate it against 0.005N sodium thiosulphate
solution
13. Record the titration value and repeat the steps10 and 11
14. Similarly, titrate the aqueous layer from other containers
15. Pipette out 10 ml of carbon tetrachloride layer in a dry and clean comical flask and add
10 ml of 10 % KI Solution.
16. Add starch solution 2 to 3 drops as an indicator and estimate concentration of iodine by
titrate with 0.1N sodium thiosulphate solution. Indicators add just before end point.
17. Repeat the step 15 and 16 till get constant burette reading.
18. Similarly, titrate other cartoon tetrachloride solution as step 15 to 17
19. Take all readings carefully
20. Calculate concentration of iodine in both phases i.e. aqueous and organic phase.
Fig.6 Titration of Aq. Layer
Fig.7 Titration of Organic Layer

Note- color change of starch indicator at end point (deep blue to light yellow)
Table: 6 Different composition of iodine solution
S. No. Container Composition
1 A 25 ml stock solution + 100 ml DW
2 B 10 ml stock solution + 10 ml CCl4 + 100 ml DW
3 C 10 ml stock solution + 20 ml CCl4 + 100 ml DW
Observation
Table: 7 Titration of Aq. Layer
S. Container Volume Burette Volume of 0.005N Normality of
No. V2 (ml) Reading Sodium thiosulphate Iodine in Aq.
Initial Final consumed in ml (V1) Phase (N2)
1 A 10
2 B 10
3 C 10
Table: 8 Titration of Organic layer

S. Container Volume Burette Volume of 0.1N Normality of
No. V2 (ml) Reading Sodium thiosulphate Iodine in Org.
Initial Final consumed in ml (V1) Phase (N2)
1 A 10
2 B 10
3 C 10
Calculation
Container A
For Aq. Layer
N1 V1 (Sodium Thiosulphate) = N2 V2 (Iodine)
N1= 0.005N V1= volume consumed of sodium thiosulphate V2 = 10 ml N2 =?
So, N2 = N1 V1 / V2
N2 = ……… mole/L
For Organic Layer
So, N2 = N1 V1 / V2
K = Corg. / Caq.
For Bottle A, K = N2 in org. layer / N2 in Aq. Layer
Container B
For Aq. Layer
So, N2 = N1 V1 / V2
For Organic Layer
So, N2 = N1 V1 / V2
K = Corg. / Caq.
For Bottle B, K = N2 in org. layer / N2 in Aq. Layer
Container C
For Aq. Layer
So, N2 = N1 V1 / V2
For Organic Layer
So, N2 = N1 V1 / V2
K = Corg. / Caq.
For Bottle C, K = N2 in org. layer / N2 in Aq. Layer
Result: Partition coefficient value of Iodine in carbon tetra chloride and water was determined
and found to be ………………………………
1. What is the meaning of partition co efficient?

A partition coefficient is the ratio of the concentration of a substance in one medium or phase
(C1) to the concentration in a second phase (C 2) when the two concentrations are at
equilibrium; that is, partition coefficient = (C1/C2)equil.
2. What is the significance of partition coefficient?

Partition coefficients are useful in estimating the distribution of drugs within the body, as it
gives a measure of a solute's hydrophobicity and a proxy for its membrane permeability
3. What is the unit of partition coefficient?

A partition coefficient essentially has no units (has units of concentration/concentration) and
is typically defined at concentrations far from saturation.
4. What is the use of separating funnel?

A separator funnel is used to separate immiscible liquids. When two immiscible liquids are
placed in a separator funnel, two layers are seen. The denser solvent will be the bottom layer.
Most halogenated solvents are denser than water; most non-halogenated solvents are less
dense than water
5. Does temperature affect partition coefficient?

Partition coefficient generally decreases with temperature. This may be due to increased
solubility of solute in water with temperature rise.
Experiment No. 05
Aim: To determine % composition of NaCl in a solution using phenol water system by CST
(critical solution temperature) method
Requirements: beaker, glass rod, volumetric flask, NaCl, Phenol, graph paper, water bath,
thermometer etc.
Theory: Conjugate solutions (a system of liquids, each partially miscible in the other, existing
with a common interface, consisting of a saturated solution of one in the other ) are defined as the
two solutions of different compositions existing in equilibrium with one another. At particular
temperature, the conjugate solutions become completely miscible with one another. The
temperatures at which two conjugate solutions are soluble giving a single layer are called
"Critical Solution Temperature" [CST] or Consolute temperature. This is the characteristic
of a particular system and is influenced very much by presence of impurities. The determination
of CST may therefore be used for testing the purity of phenol and other substances.
For phenol-water system the CST is 66.8 °C in a two-component system if a third substance is
added the CST increases, For example, if sodium chloride is added to phenol-water system,
there is an increase in CST because NaCl is more soluble in water. The increase in CST is
directly proportional to the concentration of sodium chloride.
From this the unknown concentration of sodium chloride can be detected. In this study, the
unknown concentration of sodium chloride will be determined by CST method.
Procedure
1. Prepare 100 ml of 1% NaCl in water and this serve as the stock solution. Using this stock
solution prepare 0.1, 0.2, 0.3, 0.4, 0.5, 0.6, 0.7, 0.8, 0.9 and 1% sodium chloride solution.
Table: 9 Different composition of NaCl solution
Desired Conc. Of Volume of stock Water Total Volume

NaCl solution (1%) in (ml) (ml)
(ml)
0.1 % 1 9 10
0.2 % 2 8 10
0.3 % 3 7 10
0.4 % 4 6 10
0.5 % 5 5 10
0.6 % 6 4 10
0.7 % 7 3 10
0.8 % 8 2 10
0.9 % 9 1 10
1.0 % 10 0 10
Unknown Unknown Up to 10 10
2. To 10ml of each of these solutions in a separate transition tube and add 2ml of phenol to
all the tubes.
3. Heat the mixture on water bath and note the temperature at which the mixture becomes
one layer in all the tubes (turbidity disappears).
4. Then cool the all the tubes and note at what temperature the turbidity reappears. i.e.
temperature at which turbidity appears and disappear should be noted. (Take the avg.)
5. Similarly, take 10ml of the given unknown sample. Add 2ml of phenol. Find out the CST
by the above method.
6. Graph: plot a graph by taking percentage on X axis and CST on Y axis. A straight line
will result.
7. Using the graph read the composition of unknown.
Observation
Table: 10 determination of CST for Phenol water system
Conc. Of NaCl Temp. at which Temp. at which CST in (oC)
turbidity turbidity t = (t1 + t2) / 2
disappears (oC) appears (oC)
t2 t1
0.1 %
0.2 %
0.3 %
0.4 %
0.5 %
0.6 %
0.7 %
0.8 %
0.9 %
1.0 %
Unknown
Find CST of unknown sample:

Table: 11 % Composition of NaCl vs CST
X-Axis Y-Axis
(% Composition) (CST) in (oC)
0.1 %
0.2 %
0.3 %
0.4 %
0.5 %
0.6 %
0.7 %
0.8 %
0.9 %
1.0 %
Unknown
Result:
i. CST of unknown sample = ………………………..
ii. Percentage composition of unknown sample of sodium chloride solution (from
graphical method) = ………………. %
1. Define CST.
the temperature at which complete miscibility is reached as the temperature is raised or in
some cases lowered —used of two liquids that are partially miscible under ordinary
conditions.
2. What are immiscible liquid?

Oil and water are two liquids that are immiscible – they will not mix together. Liquids tend to
be immiscible when the force of attraction between the molecules of the same liquid is
greater than the force of attraction between the two different liquids.
3. How does impurity like NaCl affect the CST of phenol-water system?
Sodium chloride is soluble only in water and not in phenol. Therefore, it will raise the CST
of phenol-water system. In this experiment, the miscibility temperatures for various mixtures
of phenol and aqueous solutions of sodium chloride are determined.
4. What is the effect of addition of salt on critical solution temperature?

The presence of salt in the solution will shift its LCST, typically to a lower temperature.
Experiment No. 06
Aim: To determine surface tension of given sample by drop count and drop weight method.
Requirements
Stalagmometer, water, density bottle, beaker, weighing balance, pinch crew clip.
Theory
Definition: the tension of the surface film of a liquid caused by the attraction of the particles in
the surface layer by the bulk of the liquid, which tends to minimize surface area.
Due to the cohesive forces, a molecule located away from the surface is pulled equally in every
direction by neighbouring liquid molecules, resulting in a net force of zero. The molecules at the
surface do not have the same molecules on all sides of them and therefore are pulled inward.
This creates some internal pressure and forces liquid surfaces to contract to the minimum area
Procedure
A. Determination of Density of water and Given Sample
1. Clean the density bottle with detergents and then with distilled water. Rinse with water
and ether and then dry.
2. Weigh an empty density bottle (W1).
3. Fill the density bottle with distilled water completely, insert the stopper and weigh again
(W2).
4. Take out the distilled water and rinse the density bottle 2-3 times with given experimental
liquid (X).
5. Fill the given experimental liquid (X) into the density bottle and record the weight again
(W3).
B. Determination of surface tension (Drop count method)

1. Clean the stalagmometer with chromic solution then with distilled water. Rinse with
water and ether and then dry.
2. Attach the stalagmometer to the burette stand in exactly vertical position.
3. Hold a beaker containing distilled water and dip the lower end of stalagmometer in it.
Suck the water just above mark “A”.
4. Allow to water to flow freely. Adjust the flow rate using pinch crew clip so that it
should deliver 15-20 drops per minute (3-4 drops in 20 second).
5. Count the no of drops falling between marks “A” to “B”.
6. Repeat the experiment 3 times for water and given sample.
7. Calculate mean value.
C. Determination of surface tension (Drop Weight method)

1. Clean the stalagmometer with chromic solution then with distilled water. Rinse
with water and ether and then dry.
3. Hold a beaker containing distilled water and dip the lower end of stalagmometer
in it. Suck the water just above mark “A”.
4. Allow to water to flow freely. Adjust the flow rate using pinch crew clip so that it
should deliver 15-20 drops per minute (3-4 drops in 20 second).
5. Weight the 20 drops of water. (by using weighing balance)
6. Weight the 20 drops of given sample. (by using weighing balance)
7. Repeat the experiment 3 times for water and given sample.
Fig.8 Stalagmometer
Observation
1. Determination of density of water and given sample
Table: 12 Density determinations (Water)
Empty Density Density bottle + Volume of Density of Water
Bottle Water density bottle Mass/Volume
(W1) gm (W2) gm (V) ml (W2-W1)/V
Water
Density of water (d1) = …………… gm/cm3
Table: 13 Density determinations (Sample)

Empty Density Density bottle + Volume of Density of Given
Bottle Given Sample density bottle Sample
(W1) gm (W3) gm (V) ml Mass/Volume
(W3-W1)/V
Given
Sampl
e
Density of Given Sample (d2) = …………… gm/cm3
2. Determination of surface tension of given sample (drop count method)
Table: 14 Surface tension determination by drop count method

Sr No of drops Surface tension Surface
No For Mean For given Mean of water tension of
water (n1) sample (n2) (γ1) given sample
(γ2)
1
2
3
3. Determination of surface tension of given sample (drop weight method)
Table: 15 Surface tension determination by drop weighed method

Sr Weight of 20 Drops Surface tension Surface
No For Mean For given Mean of water tension of
water (W4) sample (W5) (γ1) given sample
(γ2)
1
2
3
Calculation
1. Determination of density of Water and Given Sample
Density of water d1 = (W2 - W1) / V ……………………………………
Density of Given Sample d2 = (W3 - W1) / V …………………………………..
d 2 W 3−W 1
So, =
d 1 W 2−W 1
2. Determination of surface tension of given sample (drop count method)
γ 2 n1d2
=
γ 1 n2d1
γ2 = surface tension of given sample

γ1 = surface tension of water
n1 = no of drops (water)
n2 = no of drops (given sample)
d1 = density of water
d2 = density of given sample
n 1d 2
γ 2= ∗γ 1
n2d1
3. Determination of surface tension of given sample (drop weight method)
i. Weight of 20 drops (water) W4= [weight of 20drops (water) containing density

bottle] – weight of dry density bottle
ii. Weight of 20 drops (Given sample) W5 = [weight of 20drops (Given Sample)

containing density bottle] – weight of dry density bottle
γ1 W 4
=
γ2 W 5
γ2 = surface tension of given sample

W4 = Weight of 20 drops (water)
W5 = Weight of 20 drops (given sample)
W5
γ 2= ∗γ 1
W4
Result:
i. Surface tension (by drop count method) of given sample was found to be …………….
dyne/cm.
ii. Surface tension (by drop weight method) of given sample was found to be …………….
dyne/cm.
1. Define surface tension

The tension of the surface film of a liquid caused by the attraction of the particles in the
surface layer by the bulk of the liquid, which tends to minimize surface area
2. How is surface tension measured?

The surface tension is measured in dynes/cm.
3. What causes insects to float on water?

Surface tension allows objects of more density than water, like insects, to float.
4. What happens to surface tension when the temperature increases?

The surface tension decreases when the temperature increases since the net attraction
force among molecules are reduced.
5. Give an example where we can witness surface tension.

Insects walking on water and the shape of liquid droplets are ideal examples of surface
tension.
6. Can the surface tension of water support a razor blade?
Yes, a razor blade can be supported by the surface tension of water since the razorblade is
of higher density than water.
7. Which are the various types of forces due to which the liquid rises?
Forces responsible for the liquid rise are
 Cohesion
 Adhesion
 Surface tension
8. What would be the shape of the meniscus when the contact angle is greater than
90 degrees?
The shape of the meniscus when the contact angle is greater than 90 degrees would be
convex.
9. Define cohesion.
Cohesion is defined as the intermolecular attraction that acts between two same kinds of
molecules.
10. Define adhesion.

Adhesion is the intermolecular attraction acting between two different kinds of
molecules.
11. Give an example of adhesion.
Adhesion can be witnessed when the glass surface gets wet due to water. This takes place
due to the intermolecular forces between the glass and water.
Experiment No. 07
Aim: To determine HLB no of given surfactant (glyceryl monosterate) by saponification method.
Requirements: NaOH, KOH, HCl, surfactant sample, beaker, glass rod, reflux assembly,
conical flask, burette stand, weighing balance
Theory:
The HLB number scale, introduced by Griffin in 1949 was the first-ever successful attempt of a
quantitative characterization of the Polyoxyethylene non-ionic surfactants. It has often been
found that the classification of surfactants by HLB number is not helpful in enabling researchers
to predict the optimum emulsification.
HLB is short for hydrophilic-lipophilic balance. The HLB System is one of the most successful
strategies for developing stable emulsions. Griffin has established an empirical scale as a
measure of the HLB values of surfactants. It is possible to determine the optimum range for each
of surface active substance effect. The HLB system was created as a tool to make it easier to use
non-ionic surfactants.
Saponification: Saponification is the hydrolysis of an ester with NaOH or KOH to give alcohol
and sodium or potassium salt of the acid. Soaps are sodium or potassium salts of long chain fatty
acids. When triglycerides in fat/oil react with aqueous NaOH or KOH, they are converted into
soap and glycerol. This is called alkaline hydrolysis of esters. Since this reaction leads to the
formation of soap, it is called the Saponification process.
HLB Scale:
Fig.9 HLB scale
Table: 16 HLB value of different surfactant

Names of surfactants HLB
Sorbitan laurate (Span 20) 8.6
Sorbitan palmitate (Span 40) 6.7
Sorbitan stearate (Span 60 4.7
Sorbitan oleate (Span 80) 4.3
Sorbitan trioleate (Span 85) 1.8
Polyoxyethylene sorbitan laurate (Tween 20 16.7
Polyoxyethylene sorbitan palmitate (Tween 40) 15.6
Polyoxyethylene sorbitan stearate (Tween 60) 14.9
Polyoxyethylene sorbitan oleate (Tween 80) 15.0
Polyoxyethylene sorbitan trioleate (Tween 85 11.0
Procedure:
a. Preparation of 0.5N KOH alcoholic Solution
1. For preparation of 0.5N alcoholic solution, take 2.8 gm of KOH in 5ml of water.
2. And add sufficient ethanol (95%) to produce 100ml solution.
b. Preparation of 0.5N HCl

1. 1N HCl - add 36.46 gm of HCl in 1 litre of water (Molar mass of HCl = 36.46
g/mole)
2. 36.46 g of HCl is equivalent to 30.67 ml of HCl ( Volume = Mass/Density =
36.46/1.19 = 30.67)
3. Density of HCl is = 1.19 g/ml
4. Percent Concentration of Most Conc. HCl is = 37.5 %
5. 30.67 ml of HCl is equal to = (30.67)*(100/37.5) = 81.8 ml HCL
6. Hence to prepare 1N HCl - add 81.8 ml of HCl in 1000 ml of Water.
7. So. Prepare 0.5N HCl – add 40.9 ml of HCl in 100 ml of water.
c. Preparation of 0.1N KOH

1. Dissolve 5.6gm of KOH in DW and dilute of 100 ml. in volumetric flask.
d. Determination of Saponification No
1. Around 1 gram of sample (GMS) is accurately weighed and Transferred to round
bottom flask.
2. 30 ml 0.5N alcoholic potassium hydroxide is added and refluxed on a boiling water
bath for about 1 hour.
3. A blank experiment is performed in the same way but without using the sample.
4. The reaction mixtures are cooled down to room temperature and titrated against
standard 0.5N hydrochloric acid using phenolphthalein as indicator and taking colour
change pink to colorless at end point
5. Note the reading V1 for sample and V2 for blank.
e. Determination of acid value

1. Weigh accurately 1gm of stearic acid; add it to a mixture of 10ml of alcohol (ethanol)
and 10ml of ether.
2. If stearic acid does not dissolve in the solvent mixture, warm it on water bath until it
dissolves. (Note: Take care while warming, since both ether and alcohol are highly
inflammable liquids)
3. Titrate the solution of stearic acid against 0.1N KOH using phenolphthalein as the
indicator
4. Note the reading be V3.
Observation:
1. Saponification no.
a. Volume consumed of 0.5N HCl by sample (V1) = ………..ml
b. Volume consumed of 0.5N HCl by Blank (V2) = …………ml
2. Acid No
a. Volume of 0.1N KOH consumed (V3) = …………………..ml
Calculation:
1. Saponification No
(V 2−V 1 )∗Normality of HCl∗56.1
Saponification No(S )=
Amount of Sample(gm)
Saponification no (S) = ………………….

2. Acid Value
V 3∗5.61
Acid value (A) = ( )
amount of sample ∈ gm
Acid Value = …………….

3. HLB Value
S
So, HLB=20∗(1− )
A
Where,
S = Saponification No
A = acid no of fatty acid (The acid value is defined as the number of milligrams of Potassium
hydroxide/sodium hydroxide required to neutralize the free fatty acids present in one gram of
fat.)
Result: HLB value of given sample (SMG) was found to be ……………….
1. Define HLB value.

Hydrophilic–lipophilic balance (HLB) is the balance of the size and strength of the
hydrophilic and lipophilic moieties of a surfactant molecule. The HLB scale ranges from 0 to
20. In the range of 3.5 to 6.0, surfactants are more suitable for use in W/O emulsions
2. Give some example of HLB value.
Names of surfactants HLB

Sorbitan laurate (Span 20) 8.6
Sorbitan palmitate (Span 40) 6.7
Sorbitan stearate (Span 60 4.7
Sorbitan oleate (Span 80) 4.3
Sorbitan trioleate (Span 85) 1.8
Polyoxyethylene sorbitan laurate (Tween 20 16.7
Polyoxyethylene sorbitan palmitate (Tween 40) 15.6
Polyoxyethylene sorbitan stearate (Tween 60) 14.9
Polyoxyethylene sorbitan oleate (Tween 80) 15.0
Polyoxyethylene sorbitan trioleate (Tween 85 11.0
3. Define acid value.

Acid value is the mass of potassium hydroxide in milligrams that is required to neutralize
one gram of chemical substance. The acid number is a measure of the number of
carboxylic acid groups in a chemical compound, such as a fatty acid, or in a mixture of
compounds.
4. Define saponification value.

Saponification value or saponification number represents the number of milligrams of
potassium hydroxide or sodium hydroxide required to saponify one gram of fat under the
conditions specified. It is a measure of the average molecular weight of all the fatty acids
present in the sample as triglycerides.
5. Define surfactant.
a substance which tends to reduce the surface tension of a liquid in which it is dissolved.
6. What is the use of surfactant?

Surfactants play an important role in cleaning, wetting, and dispersing, emulsifying,
foaming and anti-foaming agents. Used in agrochemical formulations such as herbicides
(some), insecticides, biocides (sanitizers), and spermicides.
7. Discuss HLB scale.
8. Formula for determination of HLB value.

S
HLB=20∗(1− )
A
Where,
S = Saponification No
A = acid no of fatty acid (The acid value is defined as the number of milligrams of
Potassium hydroxide/sodium hydroxide required to neutralize the free fatty acids present
in one gram of fat.)
Experiment No.08
Aim: To determination of Freundlich and Langmuir constants using activated char coal
(determination of monolayer capacity of activated charcoal and specific surface area of
charcoal).
Requirement: water, activated charcoal, 0.5N Acetic Acid. 0.2N NaOH, Phenolphthalein,
Reagent Bottle, Beakers, Burette, Pipette, Burette Stand, Conical Flask, Funnel
Theory:
 Adsorption is the adhesion of molecules (or ions and atoms) to the surface of a solid or
liquid. The molecules accumulate only at the surface and do not enter the bulk of the
adsorbing material.
 The substance whose molecules get adsorbed at the surface is called the adsorbate.
 The substance on whose surface the process takes place is called the adsorbent.
 It is a surface phenomenon
 Desorption is the reverse process in which the adsorbed substance is removed from the
surface of the adsorbent.
Applications of Adsorption
Following are the applications of adsorption:
 Gas masks: Poisonous gases get adsorbed at the surface of the mask and prevent its
encounter when used by coal miners.
 Production of vacuum: Traces of air are adsorbed on charcoal and removed from
devices undergoing the process of evacuation.
 Removal of moisture: Silica gel pellets are used for the adsorption of moisture in
medicines and new plastic bottles in order to control humidity.
 Removal of colour: The juice extracted from cane is treated with animal charcoal for the
removal of the coloring agent in order to get a clear liquid solution
Procedure:
1. Standardization of Acetic Acid: Determine the exact normality of given acetic acid
solution by titrating 10ml (Acetic acid) against 0.2N NaOH (0.8 gm in 100ml of DW)
solution using phenolphthalein indicator. (End point: Colorless to pink).
2. Prepare following mixtures of acetic acid and distilled water in five separate dry bottles
and keep them in a water bath at room temperature.
Table: 17 Different normality solution of Acetic Acid
Bottl Volume of Volume of Total Normality of acetic

e DW (ml) acetic acid volume acid solution (N3)
(ml) (ml)
1 00 50 50 N2 =
2 10 40 50 N3 = 0.8*N2 =
3 20 30 50 N3 = 0.6*N2 =
4 30 20 50 N3 = 0.4*N2 =
5 40 10 50 N3 = 0.2*N2 =
3. Add 1gm of the activated charcoal to each of the five different dry bottles and keep them
in a water bath at room temperature.
4. Swirl the bottles for 40 min. to attain adsorption equilibrium.
5. Filter the solutions using dry filter paper into five different dry flasks.
6. And determine the effective normality of each filtered solution (N 4) by titrating 10ml
against standard 0.2N NaOH solution, using phenolphthalein indicator. (End point :
Colorless to pink)
7. Plot the graph Ce/y vs Ce. And determine slope value.
8. Determine ym (monolayer capacity) by 1/slope.
Observation:
Table: 18 Standardization of Acetic acid
S. Volume consumed Avg. (ml) Volume of acetic Conc. Of acetic
No. of 0.2N NaOH (V2) acid V1 (ml) acid (N1)
1 10 ml
Table: 19 Determination of normality of Acetic acid (N4) after addition of Activated

Charcoal
Bottle Volume consumed of Volume of Normality Normality of

No. 0.2N NaOH (V5) (acetic acid + of NaOH acetic acid
charcoal) V4 (ml) (N5) solution (N4)
1 10 ml 0.2N
2 10 ml 0.2N
3 10 ml 0.2N
4 10 ml 0.2N
5 10 ml 0.2N
Table:20 monolayer capacity determination
Bottle N3 N4 N3 – Ce = N4*60 Log Ce X= 3(N3 – x/ Log Ce

No N4 (gm/L) N4) m x/m x /m
1
2
3
4
5
N3 = Initial normality of acetic acid (before adding charcoal)

N4 = final normality of acetic acid (after adding charcoal)
Ce (Equilibrium concentration of acetic acid) = N4 * 60 gm/L (60 is MW of acetic acid)
X = amount of acetic acid adsorbed per 50ml of solution
m= mass of activated charcoal (adsorbent) = 1gm
Calculation:
1. Standardization of Acetic Acid
N1 V1 (acetic acid) = N2 V2 (NaOH)
N1 =?
N2 = 0.2N
V1 = 10 ml
V2= volume consumed of NaOH (0.2N)
N1 = N2 V2 / V1
2. Determination of normality of Acetic acid (N4) after addition of Activated Charcoal

N4 V4 (acetic acid) = N5 V5 (NaOH)
N4 =?
N5 = 0.2N
V4 = 10 ml
V5= Volume consumed of NaOH (0.2N)
N4 = N5 V5 / V4
3. Amount of acetic acid adsorbed per 50ml of solution= X

( N 3−N 4 )∗E∗50
X=
1000
E= equivalent weight of acetic acid (60)
( N 3−N 4 )∗60∗50
X=
1000
( N 3−N 4 )∗3000
X=
1000
X = 3(N3 – N4)
4. Determination of ym (monolayer capacity) : Mass of adsorbate adsorbed per gm of

adsorbent to form a monolayer (on the surface of adsorbent)
At the adsorption equilibrium
Ce 1 Ce
= +
x /m a . Ym Ym
Ce 1 1
= ∗Ce+
x /m Ym a .Ym
Ym = monolayer capacity
Ce
Plot a graph (y-axis) vs Ce (X-axis), slope of this line will be = 1/Ym
x /m
Intercept = 1/a.Ym (by keeping value of Ym calculate value of ‘a’ constant)
Ym = 1/slope
5. Determination of specific surface area of charcoal (S)

ym∗N∗A
Specific surface areaof charcoal is given by S=
M
ym= monolayer capacity

N = 6.022*1023 1/mole (Avogadro no)
Cross sectional area of acetic acid molecule (A) = 16*10-16 cm2
M= molecular weight of acetic acid (60gm/mole)
Result:
Monolayer capacity (ym) = ………………
Specific surface area (area per gram) of activated charcoal = ………………….. m2/gm
1. What are the applications of adsorption process?

Following are the applications of adsorption:
Gas masks: Poisonous gases get adsorbed at the surface of the mask and prevent its
encounter when used by coal miners.
Production of vacuum: Traces of air are adsorbed on charcoal and removed from
devices undergoing the process of evacuation.
Removal of moisture: Silica gel pellets are used for the adsorption of moisture in
medicines and new plastic bottles in order to control humidity.
Removal of colour: The juice extracted from cane is treated with animal charcoal for the
removal of the coloring agent in order to get a clear liquid solution
2. Define adsorption.
Adsorption is the adhesion of molecules (or ions and atoms) to the surface of a solid or
liquid. The molecules accumulate only at the surface and do not enter the bulk of the
adsorbing material.
3. Define term adsorbate

The substance whose molecules get adsorbed at the surface is called the adsorbate.
4. Define term adsorbent
The substance on whose surface the process takes place is called the adsorbent.
5. Define term desorption
Desorption is the reverse process in which the adsorbed substance is removed from the
surface of the adsorbent.
6. Define term absorption
Absorption is a chemical or physical phenomenon in which the molecules, atoms and
ions of the substance getting absorbed enters into the bulk phase (gas, liquid or solid) of
the material in which it is taken up. Absorption is the condition in which something gets
mixed or absorbed completely in another substance.
7. Difference between absorption and adsorption
Absorption is a separate mechanism from adsorption because molecules undergoing
absorption are soaked up by the length, not by the air. Adsorption is based on the surface
where a film of adsorbate is developed on the surface, and absorption includes the
complete volume of the absorbing agent.
8. Definition of isotherm
A line on a map or chart of the earth's surface connecting points having the same
temperature at a given time or the same mean temperature for a given period Or a line on
a chart representing changes of volume or pressure under conditions of constant
temperature.
9. Define monolayer capacity.

Mass of adsorbate adsorbed per gm of adsorbent to form a monolayer (on the surface of
adsorbent)
10. What is the meaning of activated charcoal?

Activated charcoal is made by heating charcoal in the presence of a gas. This process
causes the charcoal to develop lots of internal spaces or pores. These pores help activated
charcoal trap chemicals. Activated charcoal is commonly used to treat poisoning
Experiment No.09
Aim: To determination critical micellar concentration (CMC) of given surfactant (SLS) .
Requirements: surfactant sample, beaker, Distilled water, stalagmometer, weighing balance,
graph paper.
Theory: The CMC is an important characteristic of a surfactant. Before reaching the CMC,
the surface tension changes strongly with the concentration of the surfactant. After reaching the
CMC, the surface tension remains relatively constant or changes with a lower slope. The value of
the CMC for a given dispersant in a given medium depends on temperature, pressure, and
(sometimes strongly) on the presence and concentration of other surface active substances
and electrolytes.
Procedure:
1. 300 ml of stocks solution of surfactant SLS was prepared using distilled water having
concentration of 1mg per solution.(300 mg of SLS in 300 ml of DW = 1 mg/ml)
2. From the stocks solution strength of surfactant were prepared using distilled water i.e.
5,10,15,20,25,30,35,40,45,50 mg/L
Table: 21 Different composition of surfactant
Conc. Of Volume of Distilled Total

surfactant Stock Water Volume
(mg/L) Solution (ml) (ml)
(ml)
5 0.5 99.5 100
10 1.0 99.0 100
15 1.5 85.5 100
20 2.0 98.0 100
25 2.5 97.5 100
30 3.0 97.0 100
35 3.5 96.5 100
40 4.0 96.0 100
45 4.5 95.5 100
50 5.0 95.0 100
3. Now the surface tension of each of the strength solution was determined by using drop
weight method.
Determination of surface tension by drop weight method
4. Clean the stalagmometer with chromic solution then with distilled water. Rinse with
6. Hold a beaker containing distilled water and dip the lower end of stalagmometer in it.
Suck the water just above mark “A”.
7. Allow to water to flow freely. Adjust the flow rate using pinch crew clip so that it should
deliver 15-20 drops per minute (3-4 drops in 20 second).
8. Weight the 20 drops of water (W2). (by using weighing balance)
9. Weight the 20 drops of surfactant solutions. (by using weighing balance)
10. Repeat the experiment 3 times for water and surfactant solution.
11. Calculate mean value and surface tension for each surfactant conc.
12. Plot a graph taking concentration on X-axis and surface tension on Y-axis.
13. After reaching the CMC, the surface tension remains relatively constant or changes with
a lower slope.
14. From the graph CMC of SLS was determined.
Observation:
Table: 22 Determination of Surface tension of surfactant solution
Conc. Of Weight of 20 drops Mean Wt. of 20 drops Surface

surfactan (W2) gm (water) (W1) gm Tension of
t (mg/L) I II III Avg. surfactant
(ϒ2)
Water
5
10
15
20
25
30
35
40
45
50
Calculation:
Surface Tension of Distilled Water at RT (ϒ1)= ……………..dynes/cm
Determination of surface tension of given sample (drop weight method)
iii. Weight of 20 drops (water) W1= [weight of 20drops (water) containing density
bottle] – weight of dry density bottle
iv. Weight of 20 drops (Surfactant Solution) W2 = [weight of 20drops (Surfactant

Solution) containing density bottle] – weight of dry density bottle
γ1 W 1
=
γ2 W 2
γ2 = surface tension of surfactant solution
W1 = Weight of 20 drops (water)
W2 = Weight of 20 drops (surfactant solution)
W2
γ 2= ∗γ 1
W1
Result: Critical micellar concentration (CMC) of given surfactant (SLS) was determined
and found to be ……………….mg/ml.
1. Define CMC.
The CMC is an important characteristic of a surfactant. Before reaching the CMC,
the surface tension changes strongly with the concentration of the surfactant. After
reaching the CMC, the surface tension remains relatively constant or changes with a
lower slope. The value of the CMC for a given dispersant in a given medium depends
on temperature, pressure, and (sometimes strongly) on the presence and concentration
of other surface active substances and electrolytes.
2. Define surface tension

The tension of the surface film of a liquid caused by the attraction of the particles in
the surface layer by the bulk of the liquid, which tends to minimize surface area
3. How is surface tension measured?

The surface tension is measured in dynes/cm.
4. What causes insects to float on water?

Surface tension allows objects of more density than water, like insects, to float.
5. What happens to surface tension when the temperature increases?

The surface tension decreases when the temperature increases since the net attraction
force among molecules are reduced.
6. Give an example where we can witness surface tension.

Insects walking on water and the shape of liquid droplets are ideal examples of
surface tension.
7. Can the surface tension of water support a razor blade?

Yes, a razor blade can be supported by the surface tension of water since the
razorblade is of higher density than water.
8. Which are the various types of forces due to which the liquid rises?
Forces responsible for the liquid rise are
 Cohesion
 Adhesion
 Surface tension
9. What would be the shape of the meniscus when the contact angle is greater
than 90 degrees?
The shape of the meniscus when the contact angle is greater than 90 degrees would be
convex.
10. Define cohesion.

Cohesion is defined as the intermolecular attraction that acts between two same kinds
of molecules.
11. Define adhesion.

Adhesion is the intermolecular attraction acting between two different kinds of
molecules.
12. Give an example of adhesion.

Adhesion can be witnessed when the glass surface gets wet due to water. This takes
place due to the intermolecular forces between the glass and water.
Experiment No.10
Aim: To determine stability constant and donor acceptor ratio of PABA-Caffeine complex by
solubility method.
Requirements: Volumetric flask, beaker, conical flask , pipette, burette, burette stand with
clamp, funnel weight box, p-amino benzoic acid (PABA), sodium hydroxide, caffeine,
phenolphthalein indicator, Whatman filter paper.
Theory: Among Complexes, organic molecular complexes have innumerable applications in
pharmacy.
i. Physical State: conversion of liquid drug in to solid form (e.g. nitroglycerin is liquid
and explosive after conversion in to solid form, which is explosive proof)
ii. Volatility: complex process reduce volatility (e.g. iodine is volatile in nature but
iodine with PVP less volatile in nature)
iii. Alter chemical stability.
iv. Improved dissolution phenobarbitone is enhanced when form complex with 13
Cyclodextrins.
Complexes possess some properties, which are different from those of its components. Properties
such as solubility, light absorption, conductance, partitioning behavior and chemical reactivity
are studied to confirm the formation of complexes. For example, p Amino Benzoic Acid (PABA)
and caffeine form complexes in solution.
This results in enhanced solubility of PABA at low concentrations of caffeine. Further increase
in concentration of caffeine results in decreased solubility of PABA. Therefore, the change in the
solubility profile is taken as a criterion to decide the complexation behavior. The equation for the
formation of complex is:
PABA+ Caffeine ---------------PABA-caffeine
The interaction may be due to dipole-dipole force or hydrogen bonding between the polar
carbonyl groups of caffeine and hydrogen atom of the acid. The secondary interaction may
probably occur between the nonpolar parts of the molecules.
Procedure:
1. Prepare stock solutions of caffeine (0.1M): Weigh 1.949 gm of anhydrous caffeine and
transfer into 100 ml of volumetric flask and add distilled water to make up final volume.
2. And sodium hydroxide solution (0.025N): Dissolve 1gm of NaOH in 1000ml of
distilled water.
3. Prepare different concentrations of caffeine as per the Table below.
Table: 23 Different concentration of caffeine
Sr Vol. of caffeine Stock Distilled Conc. Of Caffeine

No Solution (ml) Water (ml) (Mole/L)
1 0 20 0
2 2 18 1
3 4 16 2
4 6 14 3
5 8 12 4
6 10 10 5
7 12 8 6
8 16 4 8
4. Fill all the 8 conc. Of caffeine solution in the different conical flask.
5. Then add equal quantities of PABA samples to each flask containing caffeine solutions.
6. Then shake all the flasks till equilibrium (approx. 30 minutes).
7. The filter the samples with Whatman filter paper.
8. Then titrate 10 ml of the sample against 0.025N sodium hydroxide (NaOH) solution
using phenolphthalein indicator.
9. End Point: pink (basic)
10. The data should be filled in the observation table.
11. Then draw the phase solubility diagram by taking concentration of caffeine on X axis and
concentration of PABA on Y axis.
12. Then calculate the Stoichiometric ratio and Complex stability constant
Fig.10 Phase solubility diagram of PABA Caffeine

Observation:
Table: 24 Titration of PABA & NaOH
Conc. Of Burette reading of NaOH Volume Conc. Of
Caffeine Initial Final Reading of NaOH PABA
(Mole/L) *102 Reading (ml) (ml) (ml) (Mole/L) *102
0
1
2
3
4
5
6
8
Calculation:
1. Determination of conc. Of PABA
N1 V1 (PABA) = N2 V2 (NaOH)
N1 =?
V1 = 10 ml (volume of titant)
N2 = 0.025N (Normality of NaOH)
V2 = volume of NaOH consumed
N2V 2
N 1=
V1
Estimation of donor acceptor ratio:
Caffeine∈ complex
Stoichimetric Ratio=
PABA∈ complex
At BC region (plateau region) conc. Of PABA and caffeine entering in to complex:

Caffeine entering∈¿ complex
Stoichimetric Ratio=
PABA entering∈¿ complex
Caffeine entering in to BC phase = caffeine at point C – Caffeine at point B
= (3.6*10-2) - (1.8*10-2)
= (1.8*10-2) mole/L
PABA entering in to BC phase = PABA total taken – PABA at point B or C
= (7.3*10-2) - (5.5*10-2)
= 1.8*10-2 mole/L
Donor acceptor Ratio or stoichiometric ratio = 1.8*10-2 mole/L / 1.8*10-2 mole/L = 1
Donor: Acceptor = 1: 1
Stability constant (K): initial linear portion of AB should be considered for the purpose of
calculation.
Conc. Of caffeine selected on X-axis = 1.0*10-2 mole/L
[ PABA−Caffeine ]
Satbility constat ( K )=
[ PABA ] [caffeine]
[PABA - Caffeine] Complex = [PABA] at (B) - [PABA] at (A)
= (5.3*10-2 ) - (4.58*10-2 )
= 0.73*10-2 mole/L
[Caffeine] Complex = [PABA – caffeine]
= 0.73*10-2 mole/L
[PABA] uncomplexed = [PABA] at point A (at solubility)
= 4.58*10-2 mole/L
[Caffeine] uncomplexed = [Caffeine] total - [Caffeine] already complexed
= caffeine chosen on X-axis - [PABA - Caffeine]
= (1.0*10-2) - (0.73*10-2)
= 0.27*10-2
Stability constant = 0.73*10-2 / (4.58*10-2) (0.27*10-2 )
= 59
Result: Stability constant (β) of PABA-Caffeine complex was determined, found to be
…………………….at donor acceptor ratio……………….
1. How to prepare 0.1M solution of caffeine.

Weigh 1.949 gm of anhydrous caffeine and transfer into 100 ml of volumetric flask and
add distilled water to make up final volume.
2. How to prepare 0.025N solution of NaOH?

Dissolve 1gm of NaOH in 1000ml of distilled water.
3. What is phase solubility diagram?

Phase solubility methods have been applied to pharmaceutical compounds to identify the solution
complexation behavior of poorly water soluble drugs or substrates with a soluble ligand.
4. Which method is used for analysis of PABA caffeine complex?

Solubility method.
5. What is the full form of PABA?

Para amino benzoic acid.
6. What is PABA used for?

PABA is taken for a disease that causes curved, painful erections (Peyronie disease), a rare
autoimmune disorder that causes skin blisters (pemphigus), hardening of skin and connective
tissue (scleroderma), and many other conditions.
Experiment No.11
Aim: To analyze copper-glycine complex by pH titration method and to calculate the formation
curve and stability constant.
Requirements: Beaker, glass rod, conical flask, pH meter, volumetric flask, glycine, cupric
chloride, distilled water, NaOH, Graph Paper
Theory:
Complexation of copper ions with Glycine can be represented by the following equation.
Cu+2 + 2NH3CH2COO- → Cu+2 + (NH2CH2COO-)2 + 2H+
Because of two protons are formed in the reaction of equation the addition of glycine to a
solution containing cupric ions should result in a decrease in pH. Titration curves can be
obtained by adding a strong base to a solution of glycine and to another solution containing
glycine and a copper salt and plotting the pH against the equivalents of base added. The results
of such a potentiometric titration are shown in the figure. The curve for the metal–glycine
mixture is well below that for the glycine alone, and the decrease in pH shows that complexation
is occurring throughout most of the neutralization range.
Fig.11 pH vs NaOH consumed (ml) for glycine and its complex
The average number of ligand groups bound per metal ion can be given by equation as
Donor acceptor ratio (n) = (Total conc. Of legend bound) / (total conc. Of metal ion)
The horizontal distance represents the amount of alkali added in the titration. This quantity is
equals to the concentration of ligand bound to metal at any pH. The total concentration of metal
ion taken initially is known. Thus, n can be calculated. The stability constant (β) and pH of free
glycine are related as
p(A) = ½ log β at n = 1
p(A) can be estimated using the equation

p(A) = pKa – pH – log([HA]initial – [NaOH])
Procedure:
1. Preparation of Glycine solution: (MW- 75.07 gm/mole, 3.34x10 -2 mole/L) weigh
250mg of glycine and transfer in to a 100ml of volumetric flask. Add distilled water and
make up volume up to the mark.
2. Complex solution (Glycine 3.34x10-2 mole/L, cupric chloride 9.45x10-3 mole/L):
weigh 250mg of glycine and 160mg of cupric chloride and transfer in to a 100ml
volumetric flask. Add distilled water and make up volume up to the mark.
3. Preparation of sodium hydroxide solution (0.25N): Dissolve 1gm of NaOH in 100ml
of distilled water.
4. Take 75ml of glycine solution in to a 250ml beaker and measure the pH of solution.
5. Add gradually 0.25N NaOH (1ml each) solution to the above glycine and periodically
measure the pH.
6. Take 75ml of complex solution in to a 250ml beaker and measure the pH of solution.
7. Add gradually 0.25N NaOH (1ml each) solution to the above glycine and periodically
measure the pH.
8. Plot a graph of pH on y-axis and no of ml of NaOH on X-axis. It will be two line graph
one for glycine solution one for complex solution.
9. After that calculate n and p[A] value by given equation at every pH point(complex
solution).
10. Plot a graph value of n (Y-axis) vs value of p[A] X-axis. That graph called formation
curve.
Fig.12 Formation curve
11. Extrapolation of formation curve determine value of n=1, for n=1 determine value of
p[A].
12. By placing the value of p[A] (at n=1) in following equation calculate value of stability
constant β.
p(A) = ½ log β
or 2 p(A) = log β
Observation:
Table: 25 Potentiometric Titration
Glycine Solution Complex solution
Volume of 0.25N pH Volume of 0.25N pH
NaOH in ml. NaOH in ml.
0 0
1 1
2 2
3 3
4 4
5 5
6 6
7 7
8 8
9 9
Calculation:
2. Determination of value of n
Total concentration of ligands bound
n=
total conc .Of metalion
Total concentration of ligand bound (NaOH) = NaOH consumed in mole/L
Total concentration of metal ion: 9.45x10-3 mole/L
0.25∗ml of NaOH consumed (per 75 ml)
Conversion of ml∈¿ mole / L=
75
Note: how to determine NaOH consumed per 75 ml of sample at any pH point? Ans: at particular
pH point calculate horizontal distance (X-axis) between glycine and glycine complex line.
(Graph: pH vs NaOH titration curve)
3. Determination of p[A] : p[A] was calculated by following equation:
p[A] = pKa – pH – log (Glycineinitial – NaOH)
pKa = 9.69
pH = from y axis of titration curve
Glycineinitial = 3.34x10-2 mole/L
NaOH = total conc. Of ligand bound (mole) (as determine during ‘n’ determination)
4. Determination of stability constant (β)
p(A) = ½ log β
Table: 26 determination of “n” and p[A]
pH ml NaOH Total legend n= Total P[A] = pKa –
solution per bound Conc. legend pH – log
75ml sample (mole/L) bound (Glycineinitial
Conc. – NaOH)
/9.45x10-3
Table: 27 Formation curve (‘n’ vs p[A])

n P[A]
(y-axis) (x-axis)
Value of p[A] =……………….at n=1
Result: stability constant (β) of copper-glycine complex was determined, found to be

…………………….at donor acceptor ratio……………….
1. Define term titration.

A titration is defined as 'the process of determining the quantity of a substance A by adding
measured increments of substance B, the titrant, with which it reacts until exact chemical
equivalence is achieved (the equivalence point).
2. What is the use of copper glycine complex?

Copper Glycine - Helps to repair connective tissue - Helps form red blood cells.
3. How to prepare 3.34x10-2 mole/L of Glycine solution?

Weigh 250mg of glycine and transfer in to a 100ml of volumetric flask. Add distilled
water and make up volume up to the mark.
4. How to complex solution?

Weigh 250mg of glycine and 160mg of cupric chloride and transfer in to a 100ml
volumetric flask. Add distilled water and make up volume up to the mark.
5. How to prepare 0.25N NaOH solution?

Dissolve 1gm of NaOH in 100ml of distilled water.
INNOVATIVE PRACTICALS
Experiment No. 12
Aim: To determine viscosity of given sample by the Ostwald viscometer.
Requirements: Ostwald viscometer, beaker, density bottle, stop watch, weighing balance,
burette stand.
Theory: The viscosity of a fluid is a measure of its resistance to deformation at a given rate. For
liquids, it corresponds to the informal concept of "thickness": for example, syrup has a higher
viscosity than water.
Viscosity quantifies the internal frictional force between adjacent layers of fluid that are in
relative motion. For instance, when a viscous fluid is forced through a tube, it flows more
quickly near the tube's axis than near its walls. Experiments show that some stress (such as
a pressure difference between the two ends of the tube) is needed to sustain the flow. This is
because a force is required to overcome the friction between the layers of the fluid which are in
relative motion. For a tube with a constant rate of flow, the strength of the compensating force is
proportional to the fluid's viscosity.
Procedure:
A. Determination of Density of water and Given Sample
1. Clean the density bottle with detergents and then with distilled water. Rinse with
2. Weigh an empty density bottle (W1).
3. Fill the density bottle with distilled water completely, insert the stopper and weigh
again (W2).
4. Take out the distilled water and rinse the density bottle 2-3 times with given
experimental liquid (X).
5. Fill the given experimental liquid (X) into the density bottle and record the weight
again (W3).
B. Determination of Viscosity
1. Clean the Ostwald viscometer with chromic solution then with distilled water.
Rinse with water and ether and then dry.
2. Attach the Ostwald viscometer to the burette stand in exactly vertical position.
Fig.13 Ostwald Viscometer
3. Fill the water in the lower bulb from tube side C.

4. Now suck the water from tube side A. slightly above the mark A.
5. Allow to water to flow freely, now keep the handy stop watch and start when
water level reaches to the mark A.
6. Note down the time taken to reach water level from mark “A” to mark “B”.
7. Repeat the experiment for three times.
8. Repeat step 3 to 7 with given sample.
Observation:
Table: 28 Determination of Density of water
(W1) gm (W2) gm (V) ml (W2-W1)/V
Water
Density of water (d1) = …………… gm/cm3
Table: 29 Determination of Density of given sample

(W1) gm (W3) gm (V) ml (W3-W1)/V
Given
Sampl
e
Density of given sample (d2) = …………… gm/cm3
Table: 30 Determination of viscosity

Sr Time taken from point “A” to “B” Viscosity of Viscosity of
No For Mean For given Mean water given sample
water (T1) sample (T2) (γ1) (γ2)
1
2
3
Calculation
A. Determination of density of Water and Given Sample
Density of water d1 = (W2 - W1) / V ……………………………………
Density of Given Sample d2 = (W3 - W1) / V …………………………………..
B. Determination of viscosity of given sample
η1 T 1d 1
=
η2 T 2d 2
η2 = viscosity of given sample
η1 = viscosity of water
T2 = time taken from point “A” to “B” (water)

T1 = time taken from point “A” to “B” (given sample)
d1 = density of water
d2 = density of given sample
T 2d 2
η 2= ∗η 1
T 1d 1
Result: Viscosity of given sample was found to be ……………………………..

1. Define term viscosity.

The viscosity of a fluid is a measure of its resistance to deformation at a given rate. For
liquids, it corresponds to the informal concept of "thickness": for example, syrup has a
higher viscosity than water.
2. What is the unit of viscosity?

The unit of viscosity is newton-second per square meter, which is usually expressed as
Pascal-second in SI units,
3. What is the use of Ostwald viscometer?

Ostwald viscometer is used to determine viscosity of Newtonian fluid. When the liquid
flow by gravity time required for the liquid to pass between two marks A and B through
the capillary tube is determined.
4. What is the role of viscosity in pharmacy?

Viscosity is an expression of the resistance to flow of a system under an applied stress. It
plays a very important role in the production of liquid pharmaceutical formulations such
as suspension, emulsion and syrups.
Let me give you an example, that how viscosity influence the emulsion system.
The emulsification process and the type of emulsion formed are influenced to some
extent by the viscosity of the two phases. Viscosity can be expected to affect interfacial
film formation because the migration of molecules of emulsifying agent to the oil/water
interface is diffusion controlled.
Droplet movement prior to coalescence (two or more the two droplets combine make a
large droplet) is also affected by the viscosity of the medium in which the droplets are
dispersed.
5. Draw the image of Ostwald viscometer.
Experiment No. 13
Aim: To study the flow properties of the given powder and effect of lubricant on flow properties.
Requirements: funnel, graph paper, scale, powder, lubricant/
Theory:
Lubricants are substances that we use in tablet and capsule formulations in order to reduce the
friction. More importantly, these substances reduce the friction between particles that we use to
make the tablet during compression. Glidants are substances that we use to increase the
flowability of a powder.
Lubrication plays a key role in successful manufacturing of pharmaceutical solid dosage forms;
lubricants are essential ingredients in robust formulations to achieve this. Although many failures
in pharmaceutical manufacturing operations are caused by issues related to lubrication, in
general, lubricants do not gain adequate attention in the development of pharmaceutical
formulations. The fundamental background on lubrication is introduced, in which the
relationships between lubrication and friction/adhesion forces.
Procedure: 0
1. Funnel was used for determination of angle of repose of given power.
2. 5 0 g m o f g i v e n p o w d e r w a s w e i g h e d .
3. The height of funnel was adjusted like tip of funnel just touch to the apex of the heap of
the powder.
4. Now free the powder to flow through the funnel. The diameter of pass powder was
measured and height of heap (h).
5. Then put the value in the following formula and calculate angle of repose ϴ.
6. Now add 5 gm of lubricant (magnesium stearate) in the 50gm of given powder. And
repeat the step 3 to 5.
tan ϴ = h / r
Fig.14 Assembly of Angle of repose determination

Table: 31 Classification of flow with angle of repose
Flow Property Angle of Repose (degrees)
Excellent 25–30
Good 31–35
Fair—aid not needed 36–40
Passable—may hang up 41–45
Poor—must agitate, vibrate 46–55
Very poor 56–65
Very, very poor >66
Observation:
Table: 32 Effect of lubricant on flow properties
Condition Sample Height of Radius of h/r Angle of Type
heap (h) cm heap (r) in cm repose ϴ of flow
Without 50gm of
lubricant Sample
With 50gm of
lubricant sample + 5
gm
lubricant
Result: Angle of repose of given powder was found to be …………….without lubricant and
…………………..with lubricant.
1. Define angle of repose.

The angle of repose or critical angle of repose, of a granular material is the steepest angle
of descent or dip relative to the horizontal plane to which a material can be piled without
slumping. At this angle, the material on the slope face is on the verge of sliding. The
angle of repose can range from 0° to 90°.
2. Define Carr’s index.

Carr Index of any solid is calculated for compressibility of a powder which is based on
true density (ρT) and bulk density (ρB), CI=100[(ρT‒ρB)/ρB]. A Carr index greater than
25 is considered to be an indication of poor flowability, and below 15, of good
flowability.
3. Define lubricant.
A lubricant is a substance that helps to reduce friction between surfaces in mutual
contact, which ultimately reduces the heat generated when the surfaces move.
4. Define glidants.
A glidants is a substance that is added to a powder to improve its flowability. A glidants
will only work at a certain range of concentrations. Above a certain concentration, the
glidants will in fact function to inhibit flowability. In tablet manufacture, glidants are
usually added just prior to compression.
5. What is the meaning of flow properties?

Powder flow, also known as flowability, is defined as the relative movement of a bulk of
particles among neighboring particles or along the container wall surface.
6. Define bulk density

Bulk density of a powder is the ratio of the mass of an untapped powder sample and its
volume including the contribution of the inter particulate void volume. Hence, the bulk
density depends on both the density of powder particles and the spatial arrangement of
particles in the powder bed.
7. Define tapped density.

The tapped density is an increased bulk density attained after mechanically tapping a
container containing the powder sample. The tapped density is obtained by mechanically
tapping a graduated measuring cylinder or vessel containing the powder sample.
8. How to enhance flow properties of powder?

The effects on flow and impedance of magnesium stearate, (colloidal silica (SiO2), and
talc were examined. These three additives are widely known to improve flow properties
9. Give example of glidants.

Ascorbyl palmitate, calcium palmitate, magnesium stearate, fumed silica (colloidal
silicon dioxide), starch and talc
10. Difference between glidants and lubricant.

Key difference between lubricant glidants and anti-adherent is that the lubricant reduces
the friction while the glidants promotes the flowability of a powder whereas the anti-
adherent provides non-sticking properties.

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Including

B.Pharm. IInd Year

Mr. Nirmal Morya Ms. Komal Verma

Assistant Professor Assistant Professor

Pranveer Singh Institute Babu Banarasi Das University

Technology (Pharmacy), Lucknow

Dr. Pranay Wal Mr. Shashi Pratap Singh

Dean, Professor Assistant Professor

Pranveer Singh Institute of Pranveer Singh Institute

Technology (Pharmacy), Technology (Pharmacy),

Dr. Pranay Wal

Shashi Pratap Singh

Dr. Pranay Wal

Shashi Pratap Singh

SHASHI PRATAP SINGH is a faculty at Pranveer Singh Institute of technology, Bhauti

2. Determination of pKa value by Half Neutralization/Henderson Hesselbalch

3. Determination of Partition co- efficient of benzoic acid in benzene and water.

4. Determination of Partition co- efficient of Iodine in CCl4 and water.

5. Determination of % composition of NaCl in a solution using phenol-water

7. Determination of HLB number of a surfactant by saponification method.

8. Determination of Freundlich and Langmuir constants using activated char coal.

9. Determination of critical micellar concentration of surfactants.

10. Determination of stability constant and donor acceptor ratio of PABA-Caffeine

12 To determine viscosity of given liquid by using Ostwald viscometer.

Fig.1 Solubility curve of different salts

1. Clean all glassware’s using detergent solution.

Table1: Observation table for solubility determination

Sr Temp Weight of Weight of Weight of Weight of Weight of

Solubility of NaCl at (…oC) = (W3 – W1 / W2 –W3) * 100

i. Solubility of NaCl at different temperature was determined.

Fig.2 solubility vs Temperature curve

VIVA-VOCE QUESTIONS AND ANSWERS

4. Effect of temperature on solubility.

5. What is the meaning of solubility curve?

Fig.3 Relationship between Ka and pKa

1. Calibrate pH meter using standard buffer tablet.

Method-2 (Half neutralization reaction)

Requirements: 0.1N NaOH, phenolphthalein indicator

Result: pKa was found to be …………… by half neutralization reaction.

VIVA-VOCE QUESTIONS AND ANSWERS

2. What is Henderson Hesselbalch equation?

4. What is half neutralization?

5. pKa of acetic acid.

The equilibrium constant K, is known as Distribution Coefficient or Partition Coefficient.

Fig.4 Titration of Organic Layer

Fig.5 Titration of Aq. Layer

Table: 4 Titration of Organic layer (Benzene)

Container Phase Conc. Of benzoic acid √Corganic Partition co

1. What is the meaning of partition co efficient?

2. What is the significance of partition coefficient?

3. What is the unit of partition coefficient?

4. What is the use of separating funnel?

5. Does temperature affect partition coefficient?

Fig.6 Titration of Aq. Layer

Fig.7 Titration of Organic Layer

Table: 8 Titration of Organic layer

1. What is the meaning of partition co efficient?

2. What is the significance of partition coefficient?