Chemical and Food Engineering Department Introduction To Engineering

BATANGAS STATE UNIVERSITY
College of Engineering, Architecture, Fine Arts

Gov. Pablo Borbon Campus II, Alangilan, Batangas City, Philippines 4200
www.batstate-u.edu.ph Telefax: (043) 300-4404 locs. 106-118
CHEMICAL AND FOOD ENGINEERING DEPARTMENT

INTRODUCTION TO ENGINEERING
Narrative Report on Webinar Entitled “Characterization

Techniques for Nanoparticles and Data Analysis”
By:
Delos Reyes, Julianne C.
ChE-2101
ChE 401: Analytical Chemistry
Professor:
Engr. Rhonalyn V. Maulion
December 2020
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INTRODUCTION
Webinars are important especially in times of pandemic where face to face
interaction is limited. Through webinars, a person can present a topic that is engaging,
relevant and informative to others. In other words, it is an online event hosted by an
organization to a selected group of individuals through their computers via the Internet. It
allows the host to share PowerPoint presentations, videos, web pages or other multimedia
content with audiences that can be located anywhere. A webinar also allows the host to
interact with its audience by asking them some questions or vice versa. Therefore, even in
times of pandemic people can still gain or expand their knowledge in various fields or
topics by attending webinars. And it is not limited to an individual’s institution or country
because a person can participate in a webinar hosted by some institutions located in other
countries.
This paper focuses in the webinar hosted by the Rayat-Bahra University entitled
“Characterization Techniques for Nanoparticles and Data Analysis” which was held last
October 13-14, 2020. The Rayat-Bahra University is a private school in Mohali, Punjab,
India which received a lot of awards and have numerous collaborations with several
industries in India. This university has six national campuses and two international
campuses. It is a two-day webinar that focuses primarily in the synthesis and
characterization of nanomaterials using different spectral techniques. The webinar has
two speakers, Dr. Ranji Garg, Head of the Chemistry Department in Rayat-Bahra
2

University, and Dr. N. Vasimalai, an Assistant Professor in Department of Chemistry in
B.S. Abdur Rahman Crescent Institute of Science and Technology.
THINGS I LEARNED FROM THE WEBINAR
The webinar started with the introduction of nanoparticles. It was said that
nanoparticles are small particles with big future. By this sentence, I learned how
important nanoparticles are. They then proceeded with its definition which stated that a
“Nano” is a Greek word which means “dwarf”, but not ideally as the same size as a
dwarf. A nanoparticle is usually defined as a particle of matter that is between 1 and 100
nanometers in diameter. Nanometer is the scale used to measure objects in the
nanoworld. It was also mentioned that nanomaterials are unique in themselves in terms of
their grains, pores, interface thickness and defects are of similar dimensions.
Nanomaterials have a large surface area but their volume is very small. It has improved
mechanical properties and is a high melting compound.
The chain of nanotechnology value is long in terms of nanomaterials,
nanointermediates, nano-enabled products and final product markets. It was also added
that nanomaterials are materials of various types at a nanoscale level. It was classified
depending on its dimensions (0D NSMs, 1D NSMs, 2D NSMs and 3D NSMs). The 0D
nanoparticles are nanomaterials in form of quantum dots, nanoparticle areas, holotubes
and nanospheres. While the 1D nanoparticles are nanomaterials that are in the form of
nanorods, nanowires, nanotubes, nanobelts, nanoribbons and hierarchial nanostructures.
3

Meanwhile, the 2D nanoparticles are nanomaterials in the form of a junction, continuous
islands, branch structures, nanoplates, nanosheets, nawalls or nanodisk. And lastly the 3D
nanoparticles are nanoballs that are in the form of dendritic sturctures, nanocoils,
nanocones, nanopillars and nanoflowers.
It was also mentioned that there is another way of classifying nanomaterials and
this depends on its overall shape. These classifications are: spherical (Nanoparticles and
Fullerenes), fibrous (Nanotubes), extremely thin layers (Nanoplates), differently
structured materials (Aggregates or Composites). Another way of classifying
nanoparticles are based on its size. Like what I’ve mentioned before, nanoparticles are
particles having sizes less than 0.1m (100nm) and then they are classified into first
generation nanoparticles and second generation nanoparticles. The first generation
nanoparticles have a size <100nm while the second generation nanoparticles have a size
<10nm. Other names of nanoparticles were also mentioned in the webinar like ultrafine
particles, clusters, nanocrystals, quantum dots, colloids, aerosols, hydrosols and
organosols.
Nanoparticles can also be synthesized by Top-down method (Destruction) and
Bottom-up method (Construction). It was mentioned that various researchers used both
methods to synthesize nanomaterials. But it was clarified that this webinar focuses in
nanoparticles not in nanomaterials hence, in order to synthesize nanopraticles the
Bottom-up and Top-down approach was used.
4

At this point, the first speaker was introduced which was Dr. N. Vasimalai. He
described nanotechnology like salt and sugar. He incorporated the concept of importance
of these substances in our everyday lives in order to make or build something bigger.
Like for example, salt and sugar are essential in cooking which we eventually eat to
survive. Without these substances, we cannot prepare food like in terms of nanoworld, a
life without nanotechnology means that we cannot do something bigger. He then
proceeded to discuss the quote by Dr. A. P.J Abdul Kalam which states that,
“Nanotechnology will play the most dominant role in the global business environment ”
which is why India’s future lies in Nanotehnology.
He then introduced the things that he will discuss for day 1 which were: X-ray
Diffraction, Scanning Electron Microscope and Transmission Electron Microscope. The
first topic he discussed is the sample preparation and data interpretation of XRD
Technique. He discussed that Wilhelm Conrad Rontgen, A German physicist, produced
and detected electromagnetic radiation in a wavelength range known as X-rays. He also
mentioned that this production and detection of X-rays earned him the Nobel Prize in
Physics in 1901. He then proceeded with the principle of XRD which he explained that it
is based on constructive interferences of monochromatic X-rays and a crystalline
samples. He added that, these X-rays are generated by cathodic ray tube which is then
filtered to produce monochromatic radiation. It is then collimated to concrete and is then
directed towards the sample. The interaction of incident rays with the sample produces
constructive interference when conditions satisfy Bragg’s Law.
5

He then discussed Bragg’s Law which states that it was used to explain the
interface pattern of X-rays scattered by crystals. This diffraction has been developed to
study the structure of all states of matter with any beam. He the mentioned that Bragg
carried out a series of experiments, the result of which he published the Bragg equation –
nƛ=2dsinɵ where it was assumed that n=1 for the first order reflection. He then showed
various XRD instruments like the Panalytical X’Pert Pro Multipurpose Powder
Diffractometer, Rigaku High-Power Powder Diffractrometer, Bruker D8 with GADDS 2-
Dimentional Detector, Bruker D8 HRXRD and the XRF.
He then explained the XRD Sample Preparation. He then gave two different
scenarios which are: if the particles are too small or wrongly grounded and if the
crystallites are not randomly oriented. He then said that if the particle is too small the
peaks get broader at the cost of the maximum intensity while in the second scenario
where the crystallites are not randomly oriented the deviating relative intensifies. He
reminded us that a fine powder is needed and showed us the difference between a coarse
and fine powder. He then showed us the right grinding device as well as the sample
loading. After that, he showed us the different background signals in terms of the SiO2,
quarts and cristobalite.
He then introduced us to the zero background holder which was an obliquely cut
single crystal either silicone or quartz. He said that the direction of the cut is chosen to
avoid any reflection sphere therefore the reflecting lattice planes are parallel to the crystal
surface. After that, he proceeded with the data interpretation which he said that we should
6

be able to find the peak position and be able to calculate the particle size. He then
mentioned the Full Width at Half Maximum (FWHM) which measures height (full
height) therefore it is full in terms of its width and half in terms of its length. He also said
that it is useful for calculation of the particle size and we will be able to tell the full width
and maximum length of one plane and other planes. He then gave us a sample problem
and showed us how to solve and graph it by the XRD Technique. He also mentioned that
the International Centre for Diffraction Data uses Joint Committee on Powder Diffraction
Standards (JCPDS) is where we can get the JCPS number which was used to solve the
problem. He then mentioned that the information in a diffraction pattern has various
aspects that needed to be considered and these are phase identification, crystal size,
crystal quality, texture and its crystal structure.
Then he discussed the sample preparation and Characterization of Scanning
Electron Microscope (SEM) and Transmission Electron Microscope (TEM) Images. The
first thing he did was differentiate the SEM from TEM. He explained that SEM is based
on scattered electron capture while TEM is based on electron transmission technique.
SEM is used to study sample surface and its morphology while TEM is used to study
detailed internal composition like morphology, magnetic domains, etc. The sample size
of SEM is thick while the sample size of TEM is thin. SEM produces low resolution
images while TEM produces high resolution images. In SEM, large amount and
multiphase sample analysis is possible while in TEM only small amount of sample can be
analyzed. SEM shows the images on monitor or picture tube while TEM shows its
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images on fluorescent screen. He also added that in SEM 3D structure can be observed
while in TEM only 2D structure can be observed and lastly, SEM is used for surfaces,
powders, polished and etched microstructures while TEM is used for imaging
dislocations, tiny ppt, grain boundaries and defects in solids.
He mentioned that in SEM Sample Preparation, there should be an appropriate
sample size where the samples can fit into its specimen chamber. He said that in coating
the specimen, nonmetals is needed to be conductive and it is done by using a device
called sputter coater. He also enumerated some conductive materials such as gold, gold-
pallidium alloy, platinum, osmium, iridium, tungsten, chromium and graphite. He then
showed us what a sputter coater looks like and proceeded with showing us what images
does the Scanning Electron Microscope produces.
He then explained to us the Energy-dispersive X-ray Spectroscopy which is
sometimes called as Energy-dispersive X-ray analysis or X-ray microanalysis is an
analytical technique used for elemental analysis or chemical characterization of a sample.
He mentioned that it relies in an interaction of some source of X-ray excitation and a
sample.
He then introduced us to the last topic which is the Transmission Electron
Microscope (TEM). He first showed us how a TEM looks like and proceeded to the TEM
sample preparation. He then showed us the TEM grids which has two types: the copper
grid and the carbon grid. He then showed us how to handle a grid and various High
Resolution TEM images. He then gave us various softwares in order to calculate the
8

particle size and these are Image J, Origin and MS Excel. He also showed us different
graphs of TEM like EDX and Line-Scan Spectra, Selected Area Electron Diffraction
Pattern.
In Day 2, Dr. Vasimalai presented to us the UV-Visible, Fluorescence and Zeta
Potential Techniques. It started with the sample preparation and data interpretation of
UV-Vis Technique. He first explained the electromagnetic radiation (EM radiation or
EMR) which refers to the waves of the electromagnetic field propagating through space
carrying electromagnetic radiant energy. He then explained the Visible Light Spectrum
which he said that it is the section of the electromagnetic radiation spectrum that is
visible to the human eye. He also mentioned that it ranges in wavelength from
approximately 400 nanometers to 700 nanometers. Then he presented the table of the
visible light spectrum which has the colors of the rainbow: Red (625nm-740nm), Orange
(590nm-625nm), Green (520nm-565nm), Blue (440nm-490nm), Indigo (420nm-440nm)
and Violet (400nm-420nm).
After that, he introduced us to Beer-Lambert Law which states that the optical
attenuation of a physical material containing a single attenuating species of uniform
concentration to the optical path length through the sample and absorptivity of the
species. Then he proceeded to electronic transitions where he enumerated the various
possible electronic transitions. He then showed us another graph which is the shift and
effect at this point, I really can’t understand what he’s saying because his voice is too low
and his microphone seems grounded. He explained to us that there are different types of
9

absorption shifts and these are the Bathochromic Shift (Red Shift), Hypsochromic Shift
(Blue Shift), Hyperchromic Effect and lastly the Hypochromic Effect.
The next topic that he discussed is the Shape and Size Dependent SPR Properties.
He first explained what SPR means. He said that it stands for Surface Plasmon
Resonance and the material for this is a semiconducting material and it is the band gap as
well as the oscillation between the electronic oxidation and the conduction band electron.
The metal surface electron is called Surface Plasma Resonance. It is an exclusive
property for metal nanoparticle. He then explained the profiles of 20nm and 80 nm of
gold. He mentioned that if it is 530-535 nm then the particle size is 20 but if it is higher
than 550 or 580 nm the particle size is 80. After that he compared the high resolution
TEM images of gold in terms of their particle size. It was seen that the higher the particle
size the more branches it obtain.
He then explained to us the Aggregation and Deaggregation of nanoparticles (Red
and Blue shift of UV-Vis Spectra). He mentioned that the spherical particle or the
selected are electron diffraction is better than single particles. After that, he showed us
how to determine the protamine. He said that the protamine is used for the patients who
will undergo surgeries. Without the protamine, the blood will clot in the surgery therefore
injecting the protamine to the patient will induce the blood flow during the surgery. The
next topic that was discussed was the Isosbestic Point. It is a specific wavelength at
which the total absorbance of the sample does not change during a chemical reaction or a
physical change of the sample.
10

Another topic was introduced and this is the Sample Preparation and Data
Interpretation of Fluorescence Technique. He said that the luminescence is the emission
of light by a substrate. It occurs when an electron returns to the electronic ground state
from an excited state and loses its excess energy as a photon. He then showed us the
Jablonski Diagram.
After that he explained that stokes shift is the difference between the maximum
wavelength of the excitation light and the maximum wavelength of the emitted
fluorescence light is a constant. He then enumerated different sensing mechanism such as
Metallophilic interaction, Interaction with metal core, Ligand-induced aggregation,
Ligand-induced charge transfer, Ligand decomposition and the Indirect approach.
He then showed us the experimental part and the calculation of quantum yield.
The first thing to do is record the UV-Vis absorbance spectrum of the solvent background
for the chosen sample (Note down the absorbance at the excitation wavelength to be
used). Next is record the fluorescence spectrum of the same solution in the 10mm
fluorescence cuvette. Calculate and note down the integrated fluorescence intensity from
the fully corrected fluorescence spectrum. After that, you should repeat the steps 1 and 2
for five solutions with increasing concentrations of the chosen sample. Then plot the
graph of integrated fluorescence intensity and absorbance. He reminded us that the result
should be a straight line with gradient and with 0 intercept.
11

He explained to us the role of capping agent for the synthesis of nanoparticles.
First was to promote the stability of the nanoparticles in a liquid medium. Second was to
alter the hydrophilicity of a particle surface to hydrophobicity. Third was to couple or
interact with analyte. Fourth was to produce building blocks for assembly and last was to
obtain functional nanoparticles.
After that, he discussed the stabilization of nanoparticles against aggregation. He
said that there are two types of stabilization the electrostatic stabilization and the steric
stabilization. In electrostatic stabilization, it is the adsorption of ions to the surface. It
creates an electrical double layer which results in a Coulombic repulsion force between
individual particles. While the steric stabilization, is all about surrounding the metal
center by layers of material that are sterically bulky.
And the last topic for this webinar is the zeta potential which he defined as the
potential observed at the shear plane. He also added that zeta potential or electro-kinetic
potential is defined as the difference in the potential between the shear plane and electro-
neutral region of motion of the solution. He explained that because of the distribution of
the charge around the particle, there is a difference in potential between the stationary
layer and the bulk solution across the diffuse layer. He also showed us the particle
charges of various surfaces in neutral water. These compounds ferric hydroxide,
aluminum hydroxide, chromium hydroxide, thorium oxide, zirconium oxide, as well as
basic dyes and basic proteins has a positive charge while the silicon dioxide, gold, silver,
12

platinum, sulfur, selenium, acidic dyes and proteins, viruses and microbes has a negative
charge.
APPLICATIONS, IMPORTANCE AND IMPLICATIONS OF THE WEBINAR
The advancement of communication technology has improved access to
information for many people all around the world. When there is a reliable internet
connection, people with communication devices can tap into the treasure trove of
information available online. People can access high quality education via the Internet.
The proliferation of the internet-based education has opened access to education to a
wider population.
Webinars offer the same advantages online classes do, namely the ability to reach
dozens or hundreds of people all around the world, with additional advantages included
as well. It is a cost-effective learning tool since students do not have to invest in
transportation or accommodation to get an education. It also offers great flexibility and
convenience since it comes with the ability to record a webinar live. Students can access
the webinar anytime that is convenient for them. Similarly, webinar presenters and
lecturers can pre-record the webinars whenever is most convenient for them.
Webinars also provide a wide variety of lessons. Many students are not able to
enroll in courses they would like to take, simply because those courses are not offered in
their institution. With webinars, students can take extra courses, regardless of the
geographical distance between where they live and the school offering the course. This
13

helps students broaden their skills, as well as their understanding of their field of interest.
This also allows students to attain new knowledge and skills that can supplement or
complement their main field of study.
In the webinar “Characterization Techniques for Nanoparticles and Data
Analysis” this are some applications of the nanoparticles. Nanoparticles are such a
wonderful innovation in today’s scenario. It gives us immense application in each and
every field. While the nanotechnology has day to day application in various fields
including pharmaceuticals and healthcare, agriculture and biotechnology,
communication, air purification and defense, robotics and space technology, water
filtration and processing, oil and gas petroleum, energy storage and energy application
and cosmetics as well.
It has versatile application for example in sports equipment, the nanotechnology
and nanoparticles reduces friction, increases hardness, reduces weight, increases its
resiliency, enhances strength to weight ratio and enhances durability. Another example is
in the field of cosmetics, nanoparticles such as zinc oxide nanoparticles plays an
important role in this field. While in the field of textiles, nanotechnology also plays an
important role since it produces a fabric with anti-static properties, wrinkle resistance,
water repellence, sensors, antibacterial or odor control as well as UV blocking.
Nanotechnology has also a great impact in the field of agriculture since it improves and
protects the crops, it enhances soil fertility, provides précised farming and increases stress
tolerance.
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Another application of Nanotechnology is in food safety and microbiology. It
increases food security, provides protection against spoilage and pathogenic
microbacteria, develops innovative products, produces nanoadditives, provides cleaning
sensors for detection of contaminants and it also improves the production of food crops.
In the field of medicine, nanoparticles provides an antimicrobial agent provides
protection against viruses, bacteria, fungi and protozoa. Nanoparticle is also a great help
in crossing the brain barriers when it was invaded by microbes and in membranes as well.
It also has a tremendous impact in wound healing, provides additional protection in PPEs
and provides friendly disinfectants. Nanoparticles and nanotechnology plays an important
role in this pandemic because it is the one being used for screening if the person has a
CoVid-19. It is also present in the things that protect us from the virus like face masks,
sanitizer, etc.
This webinar is useful for me as a Chemical Engineering student since it
introduced me to the world of nanotechnology and nanoparticles. It gave me an insight on
what our subject will be like when I take this subject in my higher year. This webinar is
also beneficial for those who are conducting and researching about this topic since it can
broaden and enlighten them on how and what should they do. This webinar also taught
me on how to interpret data using various methods which I can use in my future study
especially in my thesis paper.
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BATANGAS STATE UNIVERSITY

College of Engineering, Architecture, Fine Arts

CHEMICAL AND FOOD ENGINEERING DEPARTMENT

Narrative Report on Webinar Entitled “Characterization

Delos Reyes, Julianne C.

ChE 401: Analytical Chemistry

Engr. Rhonalyn V. Maulion

CHEMICAL AND FOOD ENGINEERING DEPARTMENT

Webinars are important especially in times of pandemic where face to face

relevant and informative to others. In other words, it is an online event hosted by an

topics by attending webinars. And it is not limited to an individual’s institution or country

campuses. It is a two-day webinar that focuses primarily in the synthesis and

characterization of nanomaterials using different spectral techniques. The webinar has

CHEMICAL AND FOOD ENGINEERING DEPARTMENT

University, and Dr. N. Vasimalai, an Assistant Professor in Department of Chemistry in

B.S. Abdur Rahman Crescent Institute of Science and Technology.

THINGS I LEARNED FROM THE WEBINAR

nanometers in diameter. Nanometer is the scale used to measure objects in the

mechanical properties and is a high melting compound.

The chain of nanotechnology value is long in terms of nanomaterials,

nanoparticles are nanomaterials in form of quantum dots, nanoparticle areas, holotubes

nanorods, nanowires, nanotubes, nanobelts, nanoribbons and hierarchial nanostructures.

CHEMICAL AND FOOD ENGINEERING DEPARTMENT

Meanwhile, the 2D nanoparticles are nanomaterials in the form of a junction, continuous

nanocones, nanopillars and nanoflowers.

Fullerenes), fibrous (Nanotubes), extremely thin layers (Nanoplates), differently

structured materials (Aggregates or Composites). Another way of classifying

generation nanoparticles and second generation nanoparticles. The first generation

particles, clusters, nanocrystals, quantum dots, colloids, aerosols, hydrosols and

Nanoparticles can also be synthesized by Top-down method (Destruction) and

nanoparticles not in nanomaterials hence, in order to synthesize nanopraticles the

Bottom-up and Top-down approach was used.

CHEMICAL AND FOOD ENGINEERING DEPARTMENT

life without nanotechnology means that we cannot do something bigger. He then

which is why India’s future lies in Nanotehnology.

Diffraction, Scanning Electron Microscope and Transmission Electron Microscope. The

Technique. He discussed that Wilhelm Conrad Rontgen, A German physicist, produced

and detected electromagnetic radiation in a wavelength range known as X-rays. He also

is based on constructive interferences of monochromatic X-rays and a crystalline

filtered to produce monochromatic radiation. It is then collimated to concrete and is then

constructive interference when conditions satisfy Bragg’s Law.

CHEMICAL AND FOOD ENGINEERING DEPARTMENT

Diffractometer, Rigaku High-Power Powder Diffractrometer, Bruker D8 with GADDS 2-

Dimentional Detector, Bruker D8 HRXRD and the XRF.

quarts and cristobalite.

CHEMICAL AND FOOD ENGINEERING DEPARTMENT

crystal quality, texture and its crystal structure.

Then he discussed the sample preparation and Characterization of Scanning

on scattered electron capture while TEM is based on electron transmission technique.

CHEMICAL AND FOOD ENGINEERING DEPARTMENT

dislocations, tiny ppt, grain boundaries and defects in solids.

He mentioned that in SEM Sample Preparation, there should be an appropriate

the specimen, nonmetals is needed to be conductive and it is done by using a device

does the Scanning Electron Microscope produces.

He then explained to us the Energy-dispersive X-ray Spectroscopy which is

sometimes called as Energy-dispersive X-ray analysis or X-ray microanalysis is an

analytical technique used for elemental analysis or chemical characterization of a sample.