ASSIGNMENT

TITRATION

PHARMACEUTICAL ANALYSIS-1 (LAB) PHC-607

PREPARED BY: GROUP B1
BP-1850103 - MEMOONA FATIMA
BP-1850149 - SALMA ABDUL HAMEED
BP-1850153 - SAMRA NOOR
BP-1850172 - SYEDA FATIMA RIZVI
BP-1850177 - TEHREEM NAZ
TITRATION:
In a titration, an unknown concentration solution is reacted with a known concentration
solution to determine its concentration.

TITRANT:

A titrant is a solution with a known concentration that is added (titrated) to another solution to
determine the concentration of a second chemical species in analytical chemistry. The titrant is
also known as the reagent, titrator or standard solution.

TITRAND:

During a titration the analyte or titrand is the species of interest. It is feasible to determine the
analyte concentration by reacting a known concentration and volume of titrant with the analyte.

INDICATOR:

A suitable indicator is used to detect the titration's end point. Indicators are weak acids or bases
whose hue in solution is proportional to their degree of ionization. Between ionized and
unionized forms, the indicator changes color. The color of an acid–base indicator (such as
phenolphthalein) changes with the ph. Examples:

• In an acidic media, methyl orange turns red and in a basic medium, it turns yellow.
• Phenolphthalein is colorless at pH 8.5 and becomes pink to dark red at pH 9.0.

EQUIVALENCE POINT:

In a titration mixture, the Equivalence Point is the point at which the chemical reaction stops.

END POINT:

The color shift that occurs at the end of a titration called the endpoint.

INFLECTION POINT:

An inflection point is the highest slope on the titration curve, and it is considered the
equivalency point. In order to determine the equivalency point, the titration curve must have
an inflection point.

CORRECTING FACTOR:

It is a mathematical modification made to a calculation to account for differences in either the

sample or the measurement method.
TITER FACTOR:

The titer is defined as the ratio of a volumetric solution's nominal concentration to its actual
concentration. The determined factor is subsequently applied to the titrant as a correction
factor. The nominal concentration is multiplied by the titer's measured value.

STANDARDIZATION:
The process of determining the exact concentration (molarity) of a solution is known as
standardization. Titration is an analytical process that is frequently used in standardization. A
titration involves reacting an exact volume of one drug with a known amount of another
substance.
PRIMARY STANDARD SOLUTION:

Primary standards are commonly employed in titrations and other analytical procedures to
determine an unknown concentration. A primary standard is a soluble solid chemical that is
extremely pure, has a constant formula that does not change when exposed to the atmosphere
and has a high molar mass.

Examples:

Oxalic acid, potassium hydrogen thalate, potassium bromate, sodium chloride, and others are
examples.

Characteristics:

A primary standard solution should have the following characteristics:

• It should be readily available and inexpensive.

• Be as pure as possible.
• During weighing the compound must remain unmodified in the air which means it must
not absorb moisture and CO2 from the air and must not oxidized by air.
• Have a reasonably big molar mass (to reduce weighing error) and be soluble (in the solvent
used and under the conditions used, to make the solution).

SECONDARY STANDARD SOLUTION:

It is a solution with a known concentration that is derived from a primary standard. It is a

solution that is tailored to a certain analysis. Analytical equipment and procedures are
calibrated using secondary standard solutions.

Examples:

NaOH, H2SO4, and KMnO4 are among examples.

Characteristics:

• These are not pure solutions.

 • The purity of a secondary standard is lower than that of a primary standard.
• These are less chemically stable and reactive than primary standards. As a result, these
substances may get polluted.
• Secondary standards are hygroscopic in nature.

EXPRESSIONS FOR CONCENTRATION:

The following expressions of concentration are given below:

1-MOLARITY:

Molarity is defined as amount of moles of compound dissolved in an amount of solvent. Its

unit is moles/liter.

Formula:
𝑨𝒎𝒐𝒖𝒏𝒕×𝟏𝟎𝟎𝟎
Molarity (M)= 𝒎𝒐𝒍𝒆𝒄𝒖𝒍𝒂𝒓.𝒘𝒆𝒊𝒈𝒉𝒕×𝒓𝒆𝒒.𝒗𝒐𝒍𝒖𝒎𝒆(𝒎𝒍)

2-NORMALITY:

Normality is defined as gram equivalent of solute per liter of solution. It is a unit of

concentration of a chemical solution.

Formula:
𝑨𝒎𝒐𝒖𝒏𝒕×𝟏𝟎𝟎𝟎
Normality (N)=𝒆𝒒𝒖𝒊𝒗𝒂𝒍𝒆𝒏𝒕 𝒘𝒆𝒊𝒈𝒉𝒕×𝒓𝒆𝒒.𝒗𝒐𝒍𝒖𝒎𝒆

3-MOLALITY:

Molality is defined as no of moles of solute per kilogram of solution.

Formula:
𝑨𝒎𝒐𝒖𝒏𝒕×𝟏𝟎𝟎𝟎
Molality (m)=𝒎𝒐𝒍𝒆𝒄𝒖𝒍𝒂𝒓 𝒘𝒆𝒊𝒈𝒉𝒕×𝒓𝒆𝒒.𝒗𝒐𝒍𝒖𝒎𝒆(𝒈𝒎)

4-MOLE FRACTION(X):

Mole fraction (x) of any component in a solution is the no of moles of the component divided
by total no of moles making up a solution. It is denoted by X.

Formula:
𝒏𝟐 (𝒎𝒐𝒍𝒆𝒔 𝒐𝒇 𝒔𝒐𝒍𝒖𝒕𝒆)
Mole fraction (solute)=𝒏𝟏 (𝒎𝒐𝒍𝒆𝒔 𝒐𝒇 𝒔𝒐𝒍𝒗𝒆𝒏𝒕)+𝒏𝟐(𝒎𝒐𝒍𝒆𝒔 𝒐𝒇 𝒔𝒐𝒍𝒖𝒕𝒆)

𝒏𝟏 (𝒎𝒐𝒍𝒆𝒔 𝒐𝒇 𝒔𝒐𝒍𝒗𝒆𝒏𝒕)
Mole fraction (solvent)=𝒏𝟏 (𝒎𝒐𝒍𝒆𝒔 𝒐𝒇 𝒔𝒐𝒍𝒗𝒆𝒏𝒕)+𝒏𝟐(𝒎𝒐𝒍𝒆𝒔 𝒐𝒇 𝒔𝒐𝒍𝒖𝒕𝒆)

5-PARTS PER MILLION (ppm):

This expression means parts of solute in a million parts of solution.

Formula:
𝒎𝒂𝒔𝒔 𝒐𝒇 𝒔𝒐𝒍𝒖𝒕𝒆
Ppm=𝒎𝒂𝒔𝒔 𝒐𝒇 𝒔𝒐𝒍𝒖𝒕𝒊𝒐𝒏 × 𝟏𝟎𝟔

6-PERCENT SOLUTION:

In which mass expressed in gram and volume in ml.

Formula:
𝑨𝒎𝒐𝒖𝒏𝒕 𝒐𝒇 𝒔𝒐𝒍𝒖𝒕𝒆
%solution=𝑨𝒎𝒐𝒖𝒏𝒕 𝒐𝒇 𝒔𝒐𝒍𝒖𝒕𝒊𝒐𝒏 × 𝟏𝟎𝟎

GLASSWARE USED IN TITRATION:

BURETTE:

A burette is a graduated glass tube with a tap on one end that is used
to dispense known volumes of liquid, particularly in titrations. It's a
graded glass tube with a stopcock at the bottom and a tapered
capillary tube at the outflow of the stopcock. The stopcock valve
regulates the flow of liquid from the tube to the burette tip.

PIPETTE:

It has suction bulb for safe pipetting and it also has calibration
marks.

BEAKER:

In laboratory equipment, a beaker is generally a cylindrical container

with a flat bottom.
ERLENMEYER FLASK:

An Erlenmeyer flask, also known as a conical flask or a titration flask,

is a type of laboratory flask which features a flat bottom, a conical
body and a cylindrical neck.

FUNNEL:

A funnel is a tube that is wide at the top and narrow at the bottom used
for guiding liquid or powder into small opening.

WEIGHING BALANCE:

A scale or balance is a device to measure weight or mass.

CALIBRATION OF APPARATUS

• Calibration of volumetric apparatus at specified intervals is an important task.

• Volume, weight and delivery time at calibration temperature are common parameters for
calibrations.
• Maintain constant temperature (25 +/- \(2^0\)C) during calibration and use calibrated
weights
• Read lower level of meniscus for clear liquid readings and upper level for colored solutions
readings, keeping your eye level horizontal in line with the liquid level

CALIBRATION OF GRADUATED PIPETTE

Graduated pipettes are used for measuring the amounts of liquid between 1 mL to 100 mL. A
pipette bulb is put on one side of the equipment to create a suction for the liquid. There are four
reasons why one needs to clean the pipette properly every once in a while.

• Clean apparatus will offer more accurate outcomes.

• It can be calibrated conveniently.
• The cross-contamination risk gets reduced.
• Well-maintained pipettes last longer.

The outer part of the apparatus can be easily cleaned using general lab cleaners. But one must check
the instruction manual before doing so. To clean the equipment from inside, distilled water can be
used. Along with this proper contamination cleaning must be done from time to time. This ensures
that none of the liquids gets contaminated during experiments. The importance of pipette
calibration increases due to the use of this equipment. Experts require the most accurate results
from it. Thus, it must be calibrated. For the purpose of calibration of graduated pipettes, these steps
can be followed:

• At time of calibration ensure no air bubbles are sticking to the glass walls and no water
droplets exist above the graduation mark
• Weigh a clean dry beaker.
• Deliver water from calibrated mark till it is emptied or in case of graduated pipette till the
calibrated mark.
• Repeat 3-4 times till consistent reading is obtained for weight, volume and delivery time.

CALIBRATION OF BURETTE

A burette is a narrow and long glass tube that comes with a stopcock at the base. The liquids are
poured from the above end and then the stopcock can be used to dispense a certain amount of it.
Titration experiment comes under one of the primary burette laboratory apparatus uses. It is
extremely vital to keep the apparatus clean before using. Otherwise, the droplets of the liquid will
stick to its walls, and it won’t give out accurate results. Besides this, the tip and stopcock of the
burette must be in place and working appropriately. It will help in getting the exact amount of
liquid. For calibration purposes of this equipment, these steps can be followed:

• Weigh a clean dry beaker.

• Deliver water from 0 mark to the point of calibration with tip touching the beaker wall.
• Weight of the collected water + beaker.
• Take note of the water temperature with a calibrated thermometer
• Repeat process at least 3 times
• Record the delivery time and volume for consistent results.

CALIBRATION OF VOLUMETRIC FLASK:

Unlike other glassware equipment on the list, a volumetric flask is used for mixing or preparing a
certain amount of any solution. It is crucial to clean this apparatus properly so that appropriate
quantities can be measured, and no contamination happens with the liquid. In general cases,
volumetric flasks can be cleaned with water or other cleaning agents. But a proper procedure must
be followed to avoid contamination. Plus they are kept in an inverted position to let the liquid at
the bottom drain away. A clean air stream can also be used to dry the equipment faster.

DIRECT TITRATION:

It is the most basic titration which is commonly used. In this type a titrant of known concentration
and volume is added to a substance in order to analyze it.
BACK TITRATION:
A back titration is a titration method where the concentration of an analyte is determined by
reacting it with a known amount of excess reagent. The remaining excess reagent is then
titrated with another second reagent. The second titration's result shows how much of the excess
reagent was used in the first titration thus allowing the original analyte's concentration to be
calculated. A back titration may also be called an indirect titration. The key difference between
titration and back titration is that in a titration we usually add a chemically equal amount of
standard solution to the analyte whereas in a back titration we add an excess amount of standard
solution to the analyte. A back titration is used when the molar concentration of an excess
reactant is known but the need exists to determine the strength or concentration of an analyte.
Back titration is typically applied in acid-base titrations:

• When the acid or (more commonly) base is an insoluble salt (e.g., calcium carbonate)
• When direct titration endpoint would be hard to discern (e.g., weak acid and weak base
titration)
• When the reaction occurs very slowly
• if the analyte is volatile (e.g., NH3)
• when no suitable indication method is available for a direct titration

BLANK TITRATION:
A blank titration is a titration without an analyte being present, only the solvent used in the
analyte solution.

APPLICATIONS OF TITRATION:

• Provide standard pharmacopeial method for the assay of unformulated drugs and some
excipients and some formulated drugs.
• It is used for standardization of raw materials and intermediate used in drug synthesis.

REFERENCES:

https://en.m.wikipedia.org/wiki/Titration

https://www.britannica.com/science/titration

https://www.pharmaguideline.com/2017/01/different-types-of-titrations.html?m=1

http://www.chem.latech.edu/~deddy/chem104/104Standard.htm

https://pediaa.com/difference-between-primary-and-secondary-standard-solution/

https://study.com/academy/answer/what-laboratory-glassware-is-used-in-a-titration.html

https://chrominfo.blogspot.com/2021/07/what-are-applications-of-titration.html?m=1