METHODS OF

PURIFICATION AND
QUALITATIVE AND
QUANTITATIVE ANALYSIS

CHEMISTRY AUNTHENTIC TASK

RASHMITHA K N

11 “B”
Purification of organic compounds is a fundamental step in
chemistry, essential for obtaining substances in their purest
form. Various techniques are employed based on the physical
and chemical properties of compounds. These techniques aim
to remove impurities and isolate the desired substance. Here,
we explore some commonly used purification methods.

1. Crystallization

Crystallization is a widely utilized method based on the

differences in solubility between the compound of interest and
impurities in a solvent. The compound is dissolved in a suitable
solvent at an elevated temperature and then allowed to cool
slowly. As the solution cools, crystals of the pure compound
form while impurities remain in the solution or form separate
crystals. The crystals are then filtered and dried to obtain the
purified compound.

2. Distillation

Distillation exploits differences in boiling points of compounds

to separate and purify them. Simple distillation is used when
the boiling points of the components differ significantly,
whereas fractional distillation is employed for compounds with
closer boiling points. The mixture is heated, and the vapors are
collected and condensed to obtain the purified compound.

3. Sublimation

Sublimation involves the direct conversion of a solid into vapor

without passing through the liquid phase. This technique is
suitable for substances that sublime readily under specific
temperature and pressure conditions. Heating the impure solid
causes it to sublime, leaving behind the impurities, and the
vapor is collected and condensed to obtain the pure compound.

4. Chromatography

Chromatography separates compounds based on their

differential affinities for a stationary phase and a mobile phase.
In paper chromatography, the mixture is applied to a paper
strip, and as the solvent moves up the paper, different
compounds in the mixture move at different rates, leading to
their separation. Other chromatographic techniques like
column chromatography and thin-layer chromatography
employ similar principles for purification.

5. Recrystallization

Recrystallization is similar to crystallization but involves the

repeated crystallization of a compound from a solvent. This
process further purifies the compound by dissolving it in a
minimum amount of hot solvent and allowing it to crystallize
upon cooling. The repeated cycles enhance the purity of the
substance.

6. Extraction

Extraction involves the selective transfer of a compound from

one phase to another based on solubility differences.
Commonly, liquid-liquid extraction is employed, where the
compound of interest is dissolved in a suitable solvent and
separated from impurities present in another solvent phase.
7. Drying

Drying is a crucial step after purification techniques involving

solvents. It involves removing traces of solvent to obtain the
pure compound. Techniques like vacuum drying or air drying
are used based on the compound's properties and sensitivity to
environmental factors.

8. Decantation and Filtration

Decantation and filtration are basic separation techniques used

to remove large impurities or separate insoluble solid
impurities from a liquid. Decantation involves pouring off the
liquid phase after settling, while filtration uses a porous
medium to separate solid particles from a liquid.
Qualitative Analysis of Organic Compounds

Qualitative analysis of organic compounds involves identifying

the presence or absence of specific functional groups or
elements within a compound. This process is vital in
determining the nature and composition of organic substances.

1. Preliminary Tests

The initial step involves conducting preliminary tests to

identify key functional groups. Tests such as the Flame Test for
organic compounds containing certain metals, the Bromine
Water Test for unsaturation (alkenes and alkynes), and the
Ferric Chloride Test for phenols provide initial indications of
functional groups present.

2. Solubility Tests

Solubility tests help in determining the solubility of the

compound in various solvents, providing clues about its
structure. For instance, polar compounds tend to dissolve in
polar solvents like water, while non-polar compounds dissolve
in non-polar solvents like ether or benzene.

3. Functional Group Identification

Specific functional groups can be identified using various tests:

- Alcohols: React with Lucas Reagent (HCl and ZnCl2) to form

alkyl halides. They also undergo oxidation to form carbonyl
compounds.
- Aldehydes and Ketones: Treated with Tollens' or Fehling's
reagent to give silver mirror or red precipitate, respectively.

- Carboxylic Acids: React with sodium bicarbonate to produce

effervescence due to the liberation of carbon dioxide gas.

- Amines: Form salts with acids, and their characteristic odor

can be detected.

4. Chromatographic Techniques

Chromatography aids in the separation and identification of

different components within a mixture. Techniques like
Thin-Layer Chromatography (TLC) or Gas Chromatography
(GC) are used to separate compounds based on their affinities to
stationary and mobile phases, allowing for qualitative analysis
based on retention times or Rf values.

5. Spectroscopic Methods

Sophisticated techniques like Infrared Spectroscopy (IR) and

Nuclear Magnetic Resonance (NMR) spectroscopy are
employed for detailed analysis. IR spectroscopy identifies
functional groups based on their characteristic absorption
frequencies, while NMR provides information about the
arrangement of atoms within the molecule.

6. Elemental Analysis

Determining the elemental composition through techniques

like combustion analysis helps in understanding the presence
of carbon, hydrogen, nitrogen, sulfur, and oxygen, aiding in the
determination of empirical formulas.

Quantitative analysis forms the bedrock of modern analytical

chemistry, serving as a key discipline for determining the
amounts and concentrations of substances within samples. It
encompasses a diverse array of techniques, each crucial for
precise measurements and in-depth understanding of chemical
compositions and properties.

Gravimetric Analysis

One of the fundamental pillars of quantitative analysis is

gravimetric analysis. This classical technique relies on the
precise measurement of mass to determine the quantity of an
analyte. It involves the separation and isolation of the substance
of interest in a measurable form, often as a precipitate, followed
by meticulous weighing to calculate its concentration in the
original sample.

Volumetric Analysis

Volumetric analysis, also known as titrimetry, involves the

measurement of volumes during chemical reactions. This
technique relies on the concept of titration, where a solution of
known concentration (the titrant) is added to a solution of the
substance being analyzed until the reaction reaches its
stoichiometric endpoint, allowing for the determination of the
unknown concentration.
Spectrophotometry and Colorimetry

The principles of spectrophotometry and colorimetry are

integral to quantitative analysis. These techniques involve the
measurement of the absorbance or transmission of light by
substances. By leveraging the relationship between
concentration and the amount of light absorbed, they provide
valuable insights into the quantification of substances in
solution.

Chromatographic Techniques

Chromatography, a diverse set of techniques, plays a pivotal

role in quantitative analysis. Gas chromatography (GC), liquid
chromatography (LC), and high-performance liquid
chromatography (HPLC) are instrumental in separating,
identifying, and quantifying components within complex
mixtures based on their interactions with stationary and mobile
phases.

Mass Spectrometry and Elemental Analysis

Mass spectrometry (MS) is a powerful technique used for

quantitative analysis. It measures the mass-to-charge ratio of
ions, providing information about the molecular mass and
structure of compounds. Elemental analysis, often utilizing
techniques like combustion analysis, aids in determining the
elemental composition of substances.