Introduction To Volumetric Analysis PH Analysis

PH ANALYSIS 1
UNIT II: Introduction to Volumetric Analysis
DEPARTMENT OF PHARMACY
1st YEAR 2nd SEMESTER A.Y. 2023 – 2024
VOLUMETRIC ANALYSIS  Graduated Cylinder - aka

 A method that involves the measuring/mixing cylinder
measurement of the volume of a  Volumetric Flask
solution of known concentration • Made to Deliver - will deliver the solution
which is used to determine the  Burette/Buret - used for
concentration of the analyte quantitative chemical analysis to
(unknown concentration) measure the volume of the liquid,
consist of graduated glass tube
 “standard solution” - known conc. with a stop cock known as turning
 analyte - unknown conc. plug at one end
 Pipette
 Graduated Cylinder
TITRIMETRIC ANALYSIS
 Pipette
 The concentration of a solution is TYPES OF BURETTE
determined by causing the solution  Mohr’s Burette - aka alkaline
to react with other solution of known burette; used for alkalimetry /
concentration. rubber pinch cock
 The chemical reaction must be  Geissler’s Burette - acidimetry /
known so that an equation can be glass stopper
written to represent the chemical
PRINCIPLE INVOLVED
change.
• Conventional - Quantitative Analysis
Ex: Na2CO3 + HCl = 2NaCl + H2O +
— we are performing quantitative analysis
CO2
in order for us to know the amount of
 AKA: volumetric analysis
standard solution that is required to
 When performing titration, the 2 completely react with all the samples
solutions must be enough wherein — the amount being identified is use to
no substance are present in excess. know the purity of a sample
 The volume of 2nd solution is noted — to determine the purity & estimate the
while the volume of the 1st solution conentration
will be calculated  VOLUMETRIC ANALYSIS
 Most of the time, the unit of volume —A+B=C
is in LITERS. — a solution of B, at known conc. Is
*NORMAL SOLUTION - contains the gram- added to a known volume of A, until the
equivalence of the substance that is number of equivalent of B is equal to
dissolved in 1L of solution those of A (analyte/sample). The added
— normality of the solution volume of B is measured and the
concentration of A can be calculated.
*MOLAR SOLUTION - 1 mole of the — we tend to find for equivalence point
substance that is dissolved in 1L of solution — % concentration
— talking about “volume”
 GRAVIMETRIC ANALYSIS
VOLUMETRIC APPARATUS —A+B=C
• Made to Contain - will contain the solution — an excess of B, at unknown
 Beaker concentration, is added to A so that A is
 Erlenmeyer Flask - aka completely transformed in C, that can be
conical/titration flask weighed.
CYDXIDSEED_
PH ANALYSIS 1
— talking about “weight”  Changes the color of solution in

Ex: ash content determination, water response to chemical change
content determination Ex: phenolphthlaein
SOURCES OF ERROR IN THE USE OF TERMS INVOLVED IN TITRATION

VOLUMETRIC APPARATUS STANDARDIZATION
 Improper cleaning of the apparatus  Process that is used to determine
 Parallax Error the concentration of a solution of
 Variation in Temperature known concentration by titrating with
 Air bubbles that tap primary solution
EQUIVALENCE POINT
ELEMENTS OF TITRATION  A point in titration where
The Standard Solution stochiometrically equivalent amount
 A solution whose concentration is of analyte and titrant reacts.
known.  A theoretical point that cannot be
Ex: NaCl, Silver Nitrate, Sodium Borate, determined experimentally, can only
NaCO3 estimate its position by observing
The Primary Standard some changes that is associated
 A highly purified compound that with the equivalent.
serve as a reference material in all ENDPOINT
volumetric method  Point in titration where we stop
 The accuracy of method is critically adding the titrant.
dependent on the properties of
primary standard solution:
 Chemically pure TITRATION ERROR
 Chemically Stable  A determinate error in a titration due
 Easily prepared to the difference between the
 Water soluble endpoint and the equivalence point.
 Reacts stochiometrically with the TYPES OF CHEMICAL REACTION IN
sample
TITRIMETRIC ANALYSIS
 With fairly high equivalent weigh
I. Neutralization Titration / Acid-Base
OTHERS
Titration
SECONDARY STANDARD i. Aqueous - water as solvent
 A compound whose purity has been ii. Non-aqueous - any solvents than
established by chemical analysis water
and will serve as the reference A + B = salt + water
material for titrimetric method of II. Complexometric Titration - metal-
analysis ligand complexation
ANALYTE — determine the conc. of metal
 The solution whose concentration ions (EDTA color changes)
has to be determined III. Precipitation Titration — analyte and
 Related to equivalence point titrant will react to form a precipitate
INDICATOR — the endpoint will be the
 Indicates if the equivalence point will precipitate
be reach nearly
CYDXIDSEED_
PH ANALYSIS 1
Ex: argentometric titration → silver salts will — change in size of the colloidal
form (AgNO3 + NaCl → AgCl (precipitate) + particle
NaNO3 (pink/reddish brown)
IV. REDOX Titration — LEORA & GEROA PROCEDURES
TITRATION TECHNIQUES
FOR USE IN TITRIMETRIC ANALYSIS A MANUAL TITRATION
REACTION MUST HAVE THE  Burette
FOLLOWING CONDITIONS:  Titrant
 Simple reactions which can be  Analyte
expressed by a chemical equation  Indicator
 Fast reaction (catalyst; speed up the  Processor
reaction)  Detector
 Alteration in some physical or chemical
property of the solution at the
DIFFICULTIES IN MANUAL TITRATION:
equivalence point.
 Reading the meniscus
 Indicator
 Filling of burette with titrant
 Reading the volume of the titrant
 Determination of end point
 Standardization of titrant
DETECTION OF END POINTS  Error in computation
(VOLUMETRIC ANALYSIS)
 Involves the observation of some AUTOMATIC TITRATION
property of the solution that change  Involves electrochemical sensing
in a characteristic way at or near the technique
equivalent point
PROPERTIES: APPLICATION OF TITRIMETRY IN
 Color change
PHARMACEUTICAL ANALYSIS
 Turbidity (malabnaw) changes
resulting from the formation or  Provide standard pharmacopoeial
disappearance of solid phase methods for assay of unformulated
 Electric conductivity of the solution. drugs and excipients
 Electric potential between a pair of  Used for standardizations of raw
electrodes immersed in the solution materials intermediates used in drug
 Temperature of the solution synthesis in industry.
 Certain specialist titration, such as
the Karl Fischer titration used to
THEORIES IN THE CHANGE OF COLOR
estimate water content, are widely
OF INDICATORS used in the pharmaceutical industry.
1. Physiochemical Theory
— change in color happens because
TYPES OF TITRATION
there is an ↑ or ↓ of ion conc.
↑ conc. - appearance/changes in color I. DIRECT TITRATION
↓ conc. - disappearance in color  The analyte is reacted with the titrant
2. Organic Theory after rendering its solubility in the
— change in molecular structure of titration medium
the solution
3. Colloidal Theory
CYDXIDSEED_
PH ANALYSIS 1
 Standard solution is made easy changing the chemical nature upon

directly to directly react with the which the titration reaction is based.
analyte
 Simplest type of titration
Analyte + titrant → product = endpoint
II. INDIRECT TITRATION

 The sample is converted to
intermediate product that is titrated
with the standard solution
 Analyte + reactant → intermediate

product
 IP + titrant = end point
III. RESIDUAL/BACK TITRATION

 Measured excess of the standard
solution is added to the sample to
accomplish a desired reaction and
the excess is back titrated with a 2nd
standard solution
 1st titrant (excess titrant); 2nd titrant
(back titrant)
Ex: Assay of Milk of Magnesia (Magnesium
Hydroxide)
REASONS FOR PERFORMING BACK

TITRATION:
 When the reaction between the
analyte and titrant proceeds slowly
 When the reaction between titrant
and analyte does not give a sharp
endpoint with the indicator
 When the sample or analyte cannot
be brought to solution without
CYDXIDSEED_

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PH ANALYSIS 1

UNIT II: Introduction to Volumetric Analysis

VOLUMETRIC ANALYSIS  Graduated Cylinder - aka

— talking about “weight”  Changes the color of solution in

SOURCES OF ERROR IN THE USE OF TERMS INVOLVED IN TITRATION

 Standard solution is made easy changing the chemical nature upon

Analyte + titrant → product = endpoint

II. INDIRECT TITRATION

 Analyte + reactant → intermediate

III. RESIDUAL/BACK TITRATION

REASONS FOR PERFORMING BACK

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