ultrasonic spectroscopy
DESCRIPTION
about ultrasonic spectroscopy - definition, introduction, principles,instrumentation with clear explanation,advantages,disadvantages,benefits, applications,TRANSCRIPT
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ULTRASONIC SPECTROSCOPY
A Presentation by-
B.Poojitha,
Aditya Institute Of Pharmaceutical sciences & Research
IInd M.Pharmacy , Pharmaceutical Analysis And Quality Assurance .
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What is ULTRASOUND?
IS High Frequency (above the Audible Range) which is taken to be above 20kHz.
What is USS?
USS Stands for ULTRASONIC Spectroscopy , measures the change in a Ultrasound Signal per unit distance as it propagates through a material .The interaction of the Ultrasonic and the material causes a energy loss in the wave which is specific to the material.
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What can USS be used for?
USS can be used to characterize the Density and
Viscosity of the Material .With addition Analysis it can
determine Solids loading and Particle size
distribution.
What type of materials can be measured?
USS is currently only used on Liquid and pure liquids
, mixtures of liquids ,emulsions ,slurries and soft
solids.
Why USS?
Non-destructive ,
Applicable to optically opaque materials ,
Fast data acquisition allows real time analysis to
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IntroductionUltrasonic or Ultrasound is derived from Latin word
Ultra means Beyond and Sonic means Sound .
Ultrasound is beyond the audible range having a
frequency of more than 20,000cycles per second. Is
simply spectroscopy employing SOUND WAVES
.Particularly uses a High Frequency ACOUSTIC
WAVE .
ACOUSTIC WAVE means the sense of hearing
,designed to respond .Similarly those used by
dolphins for communication and bats for navigation
.Sounds in the range 20-100kHz are commonly used .
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Much higher frequencies, in the range 1-20
MHz, are used for medical ultrasound. Such
sounds are produced by ultrasonic transducers.
These waves probe Intermolecular forces in
materials.
At higher power levels ,ultrasonic's is useful for
changing the chemical properties of substances .
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USS refers to a measurement method in which US
sound waves over a range of frequencies are pulsed
through a liquid medium .
USS is sensitive to particles with radius between
about 10nm to 1000um . The maximum particle
concentration which can be analyzed varies
between about 10 and 50wt% depending on the
nature of the system .
PURPOSE: Is to determine the frequency
dependent properties of materials like attenuation
, velocity .
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Sound waves travel Slowest through Gases , Faster
through Liquids and Fastest through Solids .
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Principle & Working
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PRINCIPLES.
Based on the measurements of two independent parameters-
a)Ultrasonic Attenuation and
b)Ultrasonic Velocity
a)Ultrasonic Attenuation: Is determined by the ENERGY LOSSES in Ultrasonic waves , which includes Absorption and Scattering contribution.
•Expressed in the terms of Viscosity of the Medium….
• Allows Analysis of Kinetics of Fast Chemical Reactions ,Microstructure of Materials including Particle sizing , Aggregation , Gelation , Crystallization and other processes and Characteristics.
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•Ultrasonic Attenuation measurement in
Heterogeneous systems ,like Emulsions or colloids
yields information on Particle size distribution.
•Can be used for Extensional rheology
measurement.
•As measurement of Attenuation do not require
High Temperature Stability of the Sample ,they can
be performed in the Large Samples.
b) Ultrasonic Velocity: Is determined by the Density
and the Elastic response of the sample. This
parameter is extremely sensitive to the molecular
organization and intermolecular interactions in the
medium and can be used to analyze a broad range
of molecular processes.
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The general principle of high-resolution
ultrasonic measurements as shown in
Figure .
1. The generated electronic signal is
transferred by the piezotransducer into
the ultrasonic wave travelling through the
sample.
2. Another piezotransducer then transfers
the received ultrasonic wave into an
electronic signal, which is subsequently
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Particle-Ultrasonic Wave
InteractionsThe four important types of interactions between
an Ultrasonic wave and a colloidal dispersion
are:
I. Intrinsic Absorption : Each of the individual
component phases of a colloidal suspension
absorbs Ultrasound as a result of
classical(viscous and thermal) and relaxation
loss mechanisms.
II.Visco-Inertial Dissipation Losses:In the
presence of an ultrasonic wave a particle
oscillates backwards and forwards because it
has a different density to that of the surrounding
liquid.
This oscillation is damped by the surrounding
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Amplitude of ultrasonic wave.
III.Thermal Dissipation Losses:Temperature of
particle periodically increases and decreases
relstive that of the surrounding liquid.
The temperature gradient which arises at the
particle surface causes a net flow of heat out of
the deoplet, which leads to a reduction in
Amplitude of ultrasonic wave.
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IV. Scattering losses.
The pulsation and oscillation of a
particle in the presence of an
ultrasonic wave causes the generation
of secondary ultrasonic wave by the
particle.
Thus, some of the ultrasonic energy
associated with the incident wave is
re-directed into different directions and
an increase in attenuation coefficient
may be detected.
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INSTRUMENTATION PARTS
A typical Ultrasonic spectrometry consists of a
Single Transmitter ,
A Single Analyzer and
A Measurement Cell.
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ULTRASONIC INSTRUMENT
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In a Resonator device, the sample to be analyzed
is placed in a thermostated measurement cell
between two parallel piezoelectric ultrasonic
transducers: a transmitter and a receiver.
A signal generator produces an electrical
sinusoidal wave of appropriate frequency and
amplitude.
This wave is applied to the transmitter where it is
converted into a sinusoidal ultrasonic wave that
propagates into the sample.
The ultrasonic wave undergoes multiple
reflections between the two transducers which
results in the formation of a stationary wave .
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The signal detected by the receiving transducer
is amplified and relayed to a signal analyzer.
The amplitude of the received signal goes
through a series of maxima and minima, due to
constructive and destructive interference, when
the frequency of the ultrasonic wave is varied.
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Lead Zirconate Titanate (PZT)
The piezoelectric material which had the widest
application as an ultrasonic transducer for medical
diagnostic applications is lead zirconate
titanate, commonly referred to as PZT, a shortened
form of the chemical symbols PbZrTi.
Crystals which acquire a charge when
compressed, twisted or distorted are said to be
piezoelectric. This provides a convenient transducer
effect between electrical and mechanical
oscillations. Quartz demonstrates this property and
is extremely stable. Quartz crystals are used for
watch crystals and for precise frequency reference
crystals for radio transmitters.
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Barium titanate, lead zirconate, and lead titanate
are ceramic materials which exhibit piezoelectricity
and are used in ultrasonic transducers as well as
microphones. If an electrical oscillation is applied to
such ceramic wafers, they will respond with
mechanical vibrations which provide the ultrasonic
sound source.
The standard piezoelectric material for medical
imaging processes has been lead zirconate titanate
(PZT).
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Technical parameters of the model
Two 1ml cells for parallel or differential sample analysis
Digitally Controlled Stirring System
Frequency Range from 2 to 18 MHz (cells with extended
frequency range are available on request)
High-Resolution & Reproducibility (down to 0.2mm/s for
Velocity and 0.2% Attenuation)
Variety of Measurement Regimes:
•Temperature Ramp Mode
•Kinetic Mode
•Titration Mode
•Multi-Frequency Mode
Temperature Range -20ºC to 120ºC (standard) and -40ºC to
150ºC (extended)
Absolute Temperature Control down to 0.01ºC
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EXTERNAL MODULES A choice of external modules: the standard 1ml
differential cells for liquids, 1 ml flow through cells for
fast continuous measurements of samples in
flow, differential 1.5 ml cells for semi-solids materials
and custom made fill in or follow-through cells 0.03
to 4 ml sample volume range.
The cells can be plugged to HR-US 102-P, HR-US
102 SS-P and HR-US 102 FT-P spectrometers.
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External Cell for the Analysis of LIQUIDS
External Cell for Analysis of SEMI-SOLIDS
External FLOW THROUGH Cell for
measurements in FLOW
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Versatile high resolution ultrasonic
spectrometer for analysis of
liquids The HR-US 102 high-resolution ultrasonic spectrometer
provides a broad range of analytical capabilities for
liquids. The spectrometer is equipped with precision
temperature controller and digital stirring system and can
perform measurements in dilute and concentrated
solutions, suspensions and emulsions in various
regimes: kinetics, temperature ramp, titrations and
others. The spectrometer is equipped with two 1ml
cells, which can be used independently or in differential
measurements.
Also available as P-model which offers extended
capabilities by allowing the user to attach external
modules.
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Versatile high resolution ultrasonic
spectrometer for analysis of
liquids with extended capabilitiesThe HR-US 102 P high-resolution ultrasonic
spectrometer has the same configuration as the HR-
US 102 with additional interface, which offers
extended capabilities by allowing user to attach
external modules such as cells for semi-solid
materials, measurements in flow, etc.
HR-US 102 P
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Ultrasonic Colloid Stability
AnalyzerThe NEW HR-US Colloid Stability Analyzer is
designed to enable the analysis of stability, shelf-life
and effects of thermal treatment of
emulsions, suspensions and other complex
formulations in R&D, product development, and
QA/QC environments of various industries, including
pharmaceutical, food and beverage, cosmetics and
personal care.
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High throughput ultrasonic
spectrometer for analysis of
liquids The HR-US 102 HTP high throughput ultrasonic
spectrometer equipped with semi-automated sample
introduction system, which allows fast
filling, emptying and cleaning of the ultrasonic cells.
Can do the measurements in continuous flow. Ideal
for routine repeatable measurements in analytical
labs.
Also available as P-model which offers extended
capabilities by allowing the user to attach external
modules.
HR-US 102 HTP
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Titration Kinetic Analyzer (TKA)The Titration Kinetic Analyzer measures micro
structural and molecular processes in liquids when
concentration of selected compounds is changed
(titration), or with time, when a chemical reaction is
started by an injection of a required compound.
This provides a valuable tool for product and
process development .
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TKA requires only 0.04 ml of sample allows cost-
effective analysis of expensive materials such as
proteins, nucleic acids and antibodies. The Titration
Kinetic Analyzer does not require any optical activity
of analyzed compounds and can analyze molecular
binding and chemical reactions in optically non-
transparent samples such as blood. In addition, the
Analyzer has the unique ability to follow
simultaneously an analyzed molecular process .
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Examples of application of TKA include
measurement of binding constants, drug
screening, enzymatic activity, kinetics of chemical
reactions and others. The device is based on the
patented principles of High-Resolution Ultrasonic
Spectroscopy and consists of sampling and
measuring modules. It is PC controlled, robotic
compatible, has flexible , the determination of grain
size in metals and quality control in carbon-fibre
composites and glued joints .
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BENEFITSMost materials are ultrasonically transparent
allowing the analysis of a broad variety of sample
types, chemical reactions and processes.
Hence, Ultrasonic analysis can now be easily
performed in
chemistry, physics, biotechnology, pharmaceuticals,
agriculture, environmental control, medicine
Modern ultrasonic cells do not have sharp corners
and can accommodate even aggressive liquids
such as strong acids or organic solvents without
evaporation in
the course of measurements sizes range from 4ml
down to 30µl.
The measurements are completely computer
controlled and results are presented in a
graphical,digital format, which is compatible with
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USES•Determination of molecular compressibility ,
•Determination of reaction rates,
•Changes in tertiary of large molecules like Proteins
,
•Aggregation
•On line monitoring for process control.
•Used in the analysis of sedimentation and
aggregation of drugs prepared using different
polymer coatings.
•Used in measurement of concentration profile and
sedimentation for suspensions in flow .
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ADVANTAGES
Ultrasonic Spectroscopy has many advantages
over other existing particle sizing technology
because it is
• Non-destructive in nature
•Non-invasive in nature
• Used to characterize systems which are
concentrated and optically opaque
•Capable of rapid measurement
DISAVDANTAGE
Is not suitable for dilute suspensions that is with
concentrations less than 1%wt.
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APPLICATIONS
a)To evaluate stability of EMULSIONS:Is a key
element for evaluation of the life-time and
Temperature conditions for storage and use of
emulsion based products .Ultrasonic's
measurements allow very simple procedures for
evaluation of the stability of Emulsion.
b)To determine particle size distribution of colloidal
systems
c)In the analysis of Micro emulsions
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•In addition, the ultrasonic velocity and attenuation
can be measured simultaneously at different
wavelengths as a function of the time for analysis
of kinetics of chemical reactions and processes.
•Analysis of enzymatic activity is an application of
this technique.
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REFERENCES
http://www.signal.uu.se/Publications/pdf/l061.pd
f
http://jbsr.pharmainfo.in/documents/vol3issue3/2
011030302.pdf
http://www.kenelec.com.au/sitebuilder/products/
files/902/processultrasoundspectroscopyforin-
situcharacterisation1.pdf
Simultaneously measuring concentrations of a
model drug and a model excipient in solution
using ultrasonic spectroscopy
Raymond R>Chen ,Todd Zelesky , Nicholoas
Ilasi , Sonja S. Sekulic
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Ultrasonic attenuation spectroscopy of
emulsions with droplet sizes greater than 10um
Andreas Richter , Tino Voigt , Sigefried
Ripperger
Dependence of Ultrasonic attenuation on the
material properties
Frank Babick , Frank Hinze , Sigefried Ripperger
Ultrasonic attenuation spectroscopy study of
flocculation in protein stabilized protein
Kyros Demetriades ,D.Julian McClements
Ultrasonic spectroscopy and X-ray Diffraction
study of ARB aluminum
K . Hirai , T. Ichitsubo , E.Matsubara and N.Tsuji
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High Resolution Ultrasonic spectroscopy for
Liquid chromatography
Ultrasonic spectroscopy : A promising tool for
material Analysis
M.S. kondawar and L.S. Untwal
Ultrasonic spectroscopy and Differential
Scanning Calorimetry of Liposomal
Encapsulated Nisin
T.Matthew Taylor , P.Michael Davidson , Barry
D>Bruce , and Jochen Weiss
http://books.google.co.in/books?id=NzF_KrMZ4
7IC&pg=PA38&lpg=PA38&dq=why+ultrasonic+s
pectroscopy+non+destructive%3F&source=bl&ot
s=dxaiP6XOnn&sig=n7rwlSvU3l5Bu7s_w8gnYX
2b7cY&hl=en&sa=X&ei=r1xcU5a7CJHMrQfgx4A
I&redir_esc=y#v=onepage&q=why%20ultrasonic
%20spectroscopy%20non%20destructive%3F&f
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