What are extraction techniques used for extraction of materials from their

sources.
Course title: Analyical Chemistry Practical
Course Code: CHM-610 2(0-2)
Submitted to: Dr. Nadia Noor
Submitted by: BS Group no 2
Members:- Amna sajid roll # 219
Saba Ashraf roll#222
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8TH Semester, Evening(A)

Government College Women University, Faisalabad.
Extraction:
Extraction is a seperation technique which is used to separate components from a mixture of compounds
and it is very first step to separate the desired natural products from raw materials.
Extraction is the method of removing active constituents from a solid or liquid by means of liquid solvent. In
this method the wanted components are dissolved by the use of selective solvents known as menstrum &
undissolved part is a marc. After the extraction unwanted matter is removed. Extracts are prepared by using
ethanol or other suitable solvent.

Extract: Extracts can be defined as preparations of crude drugs which contain all the constituents which are
soluble in the solvent.
Marc: Solid residue obtain after extraction

Menstrum: Solvent used for extraction

Following are 4 the stages of extraction of natural products from a raw

mixture;
I. the solvent penetrates into the solid matrix;
II. the solute dissolves in the solvents;
III. the solute is difused out of the solid matrix;
IV. the extracted solutes are collected.

Following are the different old and new extraction techniques used for
extraction of natural products from a mixture;
Old extraction techniques Modern extraction techniques
maceration Supercritical extraction
percolation Counter-current extraction
decoction Pressurized liquid extraction
Reflux extraction Microwave assisted extraction
Soxhlet extraction Ultrasound assisted extraction
Solvent extraction

Old extraction techniques

Maceration:
Maceration is the extraction of active in a solvent with shaking or stirring at room temperature, and after
defined period, the spent material is separated from the solution. is a very simple extraction method with
the disadvantage of long extraction time and low extraction efciency. It could be used for the extraction of
thermolabile components

Procedure:
 The material whose extraction is to be done is first ground into moderately course powder
 solid ingredients( coarse powder) are placed in a stoppered container with the whole of the solvent.
 it is allowed to stand for a period of at least 3 days (3 - 7 days) with frequent agitation, until soluble
matter is dissolved.
 The mixture is then strained (through sieves / nets), the marc pressed.
 The combined liquids are clarified/cleaned by filtration or by decantation, after standing.

Advantages:
It is a very simple extraction method

Disadvantages:
 It requires long extraction time
 it has low extraction efciency.

Applications:
 Maceration is used for the extraction of medicinal plants and are mostly applied for galenical
preparations.
 The role of such basic extraction procedure is to obtain the therapeutically desirable portion and
eliminate the inert material by treatment with a selective solvent known as menstruum.
 These techniques also play a decisive role in the qualitative and quantitative evaluation of the
extracts. The standardized extracts thus obtained are further processed for inclusion in other solid
and semisolid herbal dosage forms.
 These extracts are also used as sources of therapeutically active chemical constituents for various
dosage forms of modern medicines.

Example:
Optimization of polyphenols extraction from dried chokeberry using maceration as traditional technique.

Decoction:
Decoction is a method of extraction by boiling herbal or plant material to dissolve the chemicals of the
material, which may include stems, roots, bark and rhizomes.

Procedure :
 In this process, the crude drug is boiled in a specified volume of water for a defined time;
 After boiling it is cooled.
 It is then strained or filtered.

crude drug
boiled until cooled filtered
specific time

Advantages:
  They can be absorbed quickly
 they have the strongest action of all of the traditional types of preparation
Disadvantages:
 They need a reasonable amount of time to prepare, especially in chronic diseases
 they do not always taste pleasant
 they are not easy to transport or to store.
Applications:
 Decoction is the most common form of administration of Chinese herbal medicine.
 The decoction method is used particularly for serious and acute conditions.
 Decoctions can also be used topically as herbal baths for the whole body or for the
affected regions of the body.
 Decoction involves mashing the plant material to allow for maximum dissolution, and then
boiling in water to extract oils, volatile organic compounds and other various chemical
substances.
 Decoction can be used to make tisanes, tinctures and similar solutions.

Example:
Decoction of herbs
Decoction is the most common form of administration of Chinese herbal medicine. Examples of
herbs used in decoctions are ba zhen tang (eight treasure decoction) and bai hu tang (white tiger
decoction).

Reflux extraction:
Reflux extraction is a solid–liquid extraction process at a constant temperature with repeatable
solvent evaporation and condensation for a particular period of time without the loss of solvent.
Procedure:
 Pour liquid into the flask along with a stir bar or boiling stones.
 Use an extension clamp on the round bottomed flask to connect to the ring stand or
latticework.
 Attach the condenser, and connect the hoses so that water travels against gravity (cooling
water comes into the bottom and drains out the top).
 Circulate water through the condenser, then begin heating the flask (by using a heating
mantle, sand, water, or oil bath).
 Use an adjustable platform so the heat can be lowered and removed at the end of t Heat
so that the "reflux ring" is seen in the lower third of the condenser.
 Turn down the heat if the refluxing vapors reach higher than halfway up the condenser.he
reflux, or if something unexpected occurs.
  At the end of the reflux period, lower the heat source from the flask or raise the
apparatus.
 Keep circulating water in the condenser until the flask is just warm to the touch.
 After air cooling somewhat, the flask can be quickly cooled by immersing in a container
of tap water.
at end either
•lower heat source or continue circulation
pour liquid in flask
•raise apparatus until lukewarm

reflux ring seen in

add stir bar and remove flask from
lower side of
boiling stones apparatus
condensor

further cooling done

use extension clamp use adjustable by immersing in
for connection platform container of tap
water

circulate water
start heating
through condensor

Advantages:
 it is efficient
 it is easy to operate
 it is cost effective
 Reflux extraction is more efficient than percolation or maceration and requires less extraction
time and solvent.

Disadvantages:
 It cannot be used for the extraction of thermolabile natural products.

Applications:
 The system is widely used in herbal industries
 It is used in industrial and laboratory distillations.
 It is also used in chemistry to supply energy to reactions over a long period of time.

Example:
  Refluxing with 70% ethanol provided the highest yield of the natural bio-insecticidal
 A reflux system of extraction process was used to prepare plantcrude extract from dried and finely
ground leaves of A. paniculata.The extraction process was carried out in a small scale (50
mL),preparative scale (1 L) and large scale (20 L) reactor using 50%v/vaqueous ethanol. The
ratio of plant leaves to solvent was variedfrom 1:5, 1:7 and 1:10 at different temperatures ranging
from 60to 80 ◦C for 1–3 h. After extraction, the plant residue was filteredand supernatant was
collected by centrifugation. The supernatantwas dried by a rotary evaporator under vacuum

Percolation:
It is continuous downward displacement of the solvent through the bed of crude drug material to get extract. It
is Most frequently used to extract active ingredients in the preparation of tinctures and fluid extracts. It is the
method of short successive maceration or process of displacement.A percolator (a narrow, cone-shaped vessel
open at both ends) is generally used.

Procedure:
1. Size reduction: The drug to be extracted is subjected to suitable degree of size reduction, usually from
coarse powder to fine powder.
2. Imbibition: During imbibition the powdered drug is moistened with a suitable amount of menstruum
and allowed to stand for four hours in a well closed container.
3. Packing: After imbibition the moistened drug is evenly packed into the percolator.
4. Maceration: After packing sufficient menstruum is added to saturate the material. The percolator is
allowed to stand for 24 hours to macerate the drug.
5. Percolation: The lower tap is opened and liquid collected therein is allowed to drip slowly at a
controlled rate until 3/4th volume of the finished product is obtained.
Advantages:

 It Requires less time than maceration.

 It is efficient than maceration because it is a continuous process in which the saturated solvent is
constantly being replaced by fresh solvent.
 Extraction of thermolabile constituents can be possible.
Disadvantages :

 Requires more time than soxhalation.

 More solvent is required.
 Skilled person is required.

Applications
 Percolation can be used to predict water transport factors such as the rate of leaching, or the flow
of materials into water.
 This is most often used in agriculture to determine the movement of fertilizers or the salt content
of soil.
 The percolation is the most common procedure for the preparation of tinctures and fluid extracts.

Example:
The percolation is the most common procedure for the preparation of tinctures and fluid
extracts.
Soxhlet extraction
It is an exhaustive extraction technique widely applied to analytes that are sufficiently thermally
stable. The extraction solvent is continuously cycled though the matrix, by boiling and condensation,
with the sample being collected in the hot solvent.
Procedure:
 1. Boiling solvent vapors rise up through the larger side- arm.
2. Condensed drops of solvent fall into the porous cup, dissolving out the desired component from a
solid mixture.
3. When the smaller side-arm fills to overflowing, it initiates a siphoning action.
4. The solvent, containing the dissolved component, is siphoned into the boiler below residual solvent
then drains out of the porous cup, as fresh solvent drops continue to fall into the porous cup and the
cycle repeats . .

shiphoning
solvent siphoned
solvent boiled occurs below
into boiler
residual solvent

filling smaller drained out as

condensed side arm cause fresh solvent
siphoning action arrived

desired
vapours fall in
components cycle repeates
porous cup
dissolved out

Advantages:
 Large amount of drug can be extracted with much smaller quantity of solvent.
 Tremendous economy in terms of time, energy & ultimately financial input.
 Becomes more economical when converted into continuous extraction.
Disadvantages:
The high temperature and long extraction time in the Soxhlet extraction will increase the
possibilities of thermal degradation.
Applications:
 Soxhlet extraction has been used widely for extracting valuable bioactive compounds
from various natural sources.
 Typically, Soxhlet extraction is used when the desired compound has a limited
solubility in a solvent, and the impurity is insoluble in that solvent.
 It allows for unmonitored and unmanaged operation while efficiently recycling a small
amount of solvent to dissolve a larger amount of material.
Example:
Extraction of SVOCs from solid samples.
Modern extraction techniques

Supercritical fluid extraction:

Supercritical fluid:
For every substance, there is a critical temperature (Tc) and pressure (Pc) above which no applied pressure can
force the substance into its liquid phase. If the temperature and pressure of a substance are both higher than the
Tc and Pc for that substance, the substance is defined as a supercritical fluid.

Procedure:
The oldest typical and most common supercritical fluid extraction from solids is performed as a batch process,
with a continuous flow of SCF.

 An extraction medium (going to be SCF) stored in the feed tank and liquid SCF is pumped from a
reservoir ; it is heated and pressurized to reach the supercritical conditions.
 Supercritical SCF enters the extraction chamber where contact with crude drug bed occurs and the
more volatile substances are dissolved into the supercritical fluid.
 Solute and SCF leave extractor and extract is precipitated in separators, where SCF becomes gaseous.
 Gas is recycled by condensation before returning to liquid reservoir.
 SCF stored in feed extract precipitated here SCF became
tank in separator gaseous

liquid SCF pumped solute and SCF SCF gas recycled

from reservior leave extractor

heated and
pressurized until volatile substances
reach supercritical dissolved in SCF
situations

enters extraction contacted with

chamber drug bed

Advantages:
 Dissolving power of the SCF is controlled by pressure and/or temperature.
 SCF is easily recoverable from the extract due to its volatility.
 Non-toxic solvents leave no harmful residue.
 High boiling components are extracted at relatively low temperatures
 .Separations not possible by more traditional processes can sometimes be effected.
 Thermally labile compounds can be extracted with minimal damage as low temperatures can be
employed by the extraction.

Disadvantages:

 Elevated pressure required.

 Compression of solvent requires elaborate recycling measures to reduce energy costs.
 High capital investment for equipment.

Applications
 SFE finds expensive application in the extraction of pesticides
 Environmental samples
 Food and fragrances
 Essential oils
 Polymers and natural product
 Commercial application of the extraction process is its prohibitive capital investment
Example:
volatile oils can be extracted from a plant with low pressures (100 bar), whereas
liquid extraction would also remove lipids.
Counter-Current Extraction
A liquid-liquid extraction process in which the solvent and the process stream in contact with each other flow
in opposite directions.
Screw extractors and carousel extractors are the two type of equipments used for Counter-Current Extraction.

Procedure:

 In counter-current extraction (CCE), wet raw material is pulverized using toothed disc disintegrators
to produce fine slurry
 The material to be extracted is moved in one direction (generally in the form of fine slurry) within a
cylindrical extractor where it comes in contact with extraction solvent.
 The further the starting material moves, the more concentrated the extract becomes.
 Finally, sufficiently concentrated extract comes out at one end of the extractor while the marc
(practically free of visible solvent) falls out from the other end.
 wet raw material pulverized

fine slurry produced

analyte contacted with

extraction solvent

movement of analyte caused

concentration of extract

concentrated extract came

out from one end

marc falls out from other

end

Advantages :

 A unit quantity of the plant material can be extracted with much smaller volume of solvent as
compared to other methods like maceration, decoction, and percolation.
 CCE is commonly done at room temperature, which spares the thermolabile constituents from
exposure to heat which is employed in most other techniques.
 As the pulverization of the drug is done under wet conditions, the heat generated during comminution
is neutralized by water. This again spares the thermolabile constituents from exposure to heat.
 The extraction procedure has been rated to be more efficient and effective than Continuous hot
extraction.

Applications:
 Oil is to be extracted from soya beans in a counter current stage-contact extraction apparatus, using
hexane.
 application have been concerned with the purification and separaion of organic or biochemical
compound.
 application in inorganic chemistry seem to confined to separation of the radio-nuclides and a new
techniques for the determination of trace elements in geological material.
Example:
Extraction of DNP Amino Acids.
Pressurized Liquid Extraction
Pressurized liquid extraction is a sample preparation technique that combines elevated temperature and
pressure with liquid solvents to achieve fast and efficient extraction of the analytes from the solid matrix.
Procedure:
One of the solid-liquid extraction processes is PLE that is accomplished by following steps;

 take a extraction vessel which contains the sample at high temperature and increased pressure.
 introduce the solvent into the extraction vessel.
 The solvent under increased pressure and high temperature speeds up the extraction by
enhancing the analyte solubility in the solvent and increasing the rate of its desorption from the
sample matrix.
Advantages:

 It could basically resolve some of the drawbacks of the extraction methods that are currently
being used.
 Enhanced diffusivity of the solvent leads to increased efficiency and reduced extraction duration
Applications:

 PLE has been utilized in extraction of several bioactive compounds such as flavonoids, polyphenols and
several antioxidants compounds from natural matrices such as plants, fruits, vegetables and
microorganisms
 Additionally, PLE was utilized for acetophenones extraction
 PLE coupled with other analytical techniques that have been used in extraction and quantification of
contaminants compounds presents in several food stuffs such as fruits, vegetables, meats and cereals
Example:
PLE has been recently applied for the first time to the fractionation of carbohydrates.Lactulose was
separated from lactose with 70:30 (v/v) ethanol/water at 40 °C and 1500 psi using a commercial apparatus
(ASE-200; Dionex, Sunnyvale, CA, USA); yield was assessed by GC. PLE has also been applied for
obtaining honey fractions enriched in di- and trisaccharides for further GC analysis.

Microwave-assisted extraction
Microwave-assisted extraction (MAE) is a process of using microwave energy to heat solvents in contact
with a sample in order to partition analytes from the sample matrix into the solvent.
MAE is a conventional technique for the extraction of active components from medicinal plants, using
microwave energy to heat solvents containing samples, thereby partitioning analytes from a sample
matrix into the solvent.
Procedure:
the extraction mechanism of MAE involves three steps
1. . First, increase in temperature and pressure which results in solutes’ separation from active sites
of sample matrix;
2. secondly, the solute is released to solvent from sample matrix and
3. finally solvent gets diffused across sample matrix

causes separation of solute released to solvent gets

temperature and
solute from active slolvent from diffused across
pressure increased
sites of sample sample matrix sample matrix
Advantages:

 The main advantage of MAE is its ability to rapidly heat the sample solvent mixture, resulting in
its wide applicability for the rapid extraction of analytes, including thermally unstable substances.
 The other major advantage of MAE over the conventional extraction methods is its microwave
radiation, which enhances the evaporation of raw material residual water and eventually breaks
the plant cell walls to promote the extraction through internal diffusion
 the energy loss to the surrounding environment in MAE is very less as the heating occurs in a
selective and targeted manner.

Applications:
 Pesticide analyses
 Isolation of important in pharmaceutical compounds
 Extraction of virtually all compounds from all matrices.
 The application of microwave assisted extraction process is also for isolation and extraction
of phytoconstituents from plant material

Example:
Garicus bisporus samples and fungal spores and hyphae from other species were extracted by means of
MAE.
Ultrasound assisted extraction:
Ultrasonic-assisted extraction (UAE) is one of the modifications, where the extraction process
is assisted with the usage of ultrasound waves. Two major factors that increase the efficiency of
using ultrasound waves are cell disruption and the effective mass transfer

Quercus Infectoria galls or known as Manjakani, is one of the potential herbs that have
multiple therapeutic properties and are widely used in folklore medicine.
Procedure:
 In this study, sample Quercus Infectoria galls were used in powder form.
 Powdered Quercus Infectoria galls were immersed in the extraction solvent and the mixture was
heated on a hotplate with continuous stirring for 8 hours.
 The extraction temperature was set at 70°C, the sample-to-solvent ratio at 1:10 (sample: water)
with volume of infusion was set at 100 ml.
 The mixture was covered with aluminium foil throughout the extraction to minimize the
evaporation in order to maintain the sample-to-solvent ratio.

powdered quercus infectoria galls

immersed in extraction solvent

mixture heated on hotplate

with continuous stirring

Advantages:
 The yield obtained by this method is significantly higher as compared to the conventional
extraction system.
 probe sonication system used in this technique significantly induces the extraction efficiency to
increase the bioactive constituents yield.
 Applications
 Sonication can be used for the production of nanoparticles, such as nanoemulsions, nanocrystals,
liposomes and wax emulsions, as well as for wastewater purification
 extraction of plant oil
 production of biofuels
 crude oil desulphurization, cell disruption,
 polymer and epoxy processing, adhesive thinning, and many other processes.
 It is applied in pharmaceutical, cosmetic, water, food, ink, paint, coating, wood treatment,
metalworking, nanocomposite, pesticide, fuel, wood product and many other industries.
 Sonication can also be used to initiate crystallisation processes and even control polymorphic
crystallisations.
 It is used to intervene in anti-solvent precipitations (crystallisation) to aid mixing and isolate small
crystals.

Example:
The first application of this technique for the study of honey volatile fraction. The authors applied a USE
methodology for Greek citrus honeys and flowers. The volatile fraction both of fresh flower and honey
samples was extracted using an n-pentane/diethylether (1:2) mixture in an ultrasound water bath
apparatus, maintained at 25 °C for 10 min; the extracts were then analyzed directly by GC-FID and GC-
MS using an apolar capillary column operating at programmed temperature with helium as carrier gas.

Solvent extraction:-

Solvent extraction is a process in which compounds are separated based on their relative
solubilities. This treatment method involves using a solvent - a fluid that has the ability to
dissolve another substance.

Solvent extraction, also called liquid – liquid extraction, can be used to separate a
substance from a solution by extraction into another solvent. It can be used either to
recover a valuable substance from the original solution, or to purify the
original solvent by removing an unwanted component.

The most suitable solvents are aqueous mixtures containing ethanol, methanol, acetone,
and ethyl acetate. Ethanol has been known as a good solvent for polyphenol extraction
and is safe for human consumption.
 Two distinct approaches for LLE are possible, i.e. discontinuous LLE, where equilibrium
is established between two immiscible phases, or continuous LLE, where equilibrium
may not be established between two immiscible liquids.

Advantages of solvent extraction:-.

 Good quality extract, efficient, selective, minimized product degradation,
eliminates solvent residues
 low energy consumption, large production capacity, fast action, easy continuous
operation and ease of automation.
 It is a simple, selective, cost-effective and uncomplicated chemical process
 Disadvantages:
 Time consuming, high temperatures used may alter compounds.
 High cost, technical skills required.

Applications:
 Solvent extraction is widely employed in a variety of industries for both the
upgrading and purification of a range of elements and chemicals.
 This technology is used in applications as diverse as ore processing,
pharmaceuticals, agriculture, industrial chemicals, petrochemicals, food industry,
purification of base metals and refining of precious metals
 Solvent extraction (SX) was employed mainly as an analytical tool for the separation and
analysis of elements with very similar chemical properties. The discovery and isolation of
the lanthanide and actinide elements provided impetus for the further development of
these technologies (60).
 Solvent extraction is applied nowadays in various industries. This is a classic method of
separation and concentration of metal ions from aqueous solutions.
 applied in hydrometallurgical separation and purification of various metals

Example:
 extraction of non-ferrous metals from hydrometallurgical leach liquors.
 Extraction/Separation of Lead , Zinc , Uranium, Iron , Cadmium, Hafnium , Zirconium &
Plutonium
Discontinuous solvent extraction:-

Procedure:-
 In discontinuous extraction the most common approach uses a separating funnel.
 The aqueous sample is introduced into a large separating funnel (2 l capacity with a
Teflon stopcock) and 60 ml of a suitable organic solvent, e.g. dichloromethane, is added.
 A stopper is then placed into the top of the separating funnel and the separating funnel is
then shaken manually.
 By placing the stoppered end of the separating funnel into the palm of the hand an
inversion of the funnel can take place.
 This process is repeated for approximately 1–2 min (inverting the separating funnel
approximately 5–6 times)
 The process can also be automated by using a mechanical ‘bed-shaker’. The shaking
process allows thorough interspersion between the two immiscible solvents, thereby
maximizing the contact between the two solvent phases and hence assisting mass
transfer, and allowing efficient partitioning to occur.
 After a suitable resting period (approximately 5 min) the organic solvent is collected by
opening the stopcock and carefully running out the lower phase (assuming this to be the
organic phase) and quantitatively transferred to a volumetric flask.
 Fresh organic solvent is then added to the separating funnel and the process repeated
again. This should be done at least three times in total.
 The three organic extracts should be combined, ready for concentration.

put sample
remove lower
into separating open stopcock
phase
funnel

add organic rest for add fresh

solvent suitable time organic solvent

place stopper
repeat repeat 3 times
on the funnel

combine
shake invert
extracts
Continuous solvent extraction:-
In some cases where the kinetics of the extraction process are slow, such that the equilibrium of
the compound between the aqueous and organic phases is poor, i.e. Kd is very small, then
continuous LLE can be used.This approach can also be used for large volumes of aqueous
sample.

Procedure:-
 In this situation, fresh organic solvent is boiled, condensed and allocated to percolate
repetitively through the compound-containing aqueous sample.
 Two common versions of continuous liquid extractors are available, using either lighter-
than or heavier-than water organic solvents.
 Extractions usually take several hours, but do provide concentration factors of up to
×105. Obviously several systems can be operated unattended and in series, allowing
multiple samples to be extracted.
 Typically, a 1 l sample, pH adjusted if necessary, is added to the continuous extractor.
Then organic solvent, e.g. dichloromethane (in the case of a system in which the solvent
has a greater density than the sample), of volume 300–500 ml, is added to the distilling
flask together with several boiling chips.
 The solvent is then boiled, using a water bath, and the extraction process continues for
18–24 h. After completion of the extraction process, and allowing for sufficent cooling
time, the boiling flask is detached and solvent evaporation can then occur.
 sample added organic solvent
solvent boiled condensed
to extractor added

process
boling chips
cooled continued for boiled
added
18-24 hrs

Example:
Examples of solvent extraction are the extraction of uranium and plutonium salts from solution in
nitric acid in nuclear fuel reprocessing using kerosene as solvent, and the extraction of benzene from
reformed naphtha using sulfolane as solvent.