Minor Project Report
Minor Project Report
Minor Project Report
(A Constituent Autonomous Institute and Recognised by UGC Section 12(B) and 2(F))
Minor Project
Synthesis and Characterisation of Chitin based Nanocomposites
The assistance and help during this period of investigation has been fully acknowledged.
(Project Guide)
CERTIFICATE
The assistance and help during this period of investigation has been fully acknowledged.
(Project Guide)
DECLARATION
Aarzoo Rana
Aman
ACKNOWLEDGEMENT
We hereby acknowledge all those people who have made this project report possible and
because of whom my experience has been one that we will cherish forever. First of all,
we would like to express my sincere thanks to Dr. Sunil Dhingra, Director, University
Institute of Engineering and Technology, Kurukshetra University, Kurukshetra and Dr.
Amita Mittal, Faculty Incharge , Department of Biotechnology, for giving us this golden
opportunity to work with the enriched laboratory .We would also extend our deep
gratitude to Dr. Deepak Malik, Assistant Professor, Department Of Biotechnology,
(U.I.E.T), Kurukshetra University, Kurukshetra for permitting us to work in his laboratory
and showing immense generosity during entire course of our project. We express our
deep sense of gratitude and indebtedness to him for his constant support and inspiring
guidance.
Finally, we would like to extend a lot of thanks to my fellow lab partners for their wise and
concrete suggestion and meticulous attention which helped me to learn more about my
work. It was truly a pleasure to learn and develop research skills alongside them. We
would like to thank our friends for encouraging us and extending their cooperation in a
benefiting manner during every stage of our work. Last but not least, We owe our soulful
thanks to Almighty God and our families for endowing their immense blessings and love
on us that helped us towards the successful completion of our work.
Table of Contents
1. Introduction
2. Review of Literature
3. Materials and Methods
4. Result and Discussion
5. Conclusion
6. References
(1) Introduction
Nanotechnology can be broadly defined as, “The creation, processing, characterization, and utilization of
materials, devices, and systems with dimensions on the order of 0.1–100 nm, exhibiting novel and
significantly enhanced physical, chemical, and biological properties, functions, phenomenon, and processes
due to their nanoscale size”. Current interests in nanotechnology encompass nano-biotechnology, nano-
systems, nano-electronics, and nano- structured materials, of which nanocomposites are a significant part.
NPs are not simple molecules itself and therefore composed of three layers i.e. the surface layer, which
may be functionalized with a variety of small molecules, metal ions, surfactants and polymers, the shell
layer, which is chemically different material from the core in all aspects, and the core, which is essentially
the central portion of the NP and usually refers the NP itself . Owing to such exceptional characteristics,
these materials got immense interest of researchers in multidisciplinary fields. Presently, different metallic
nanomaterials are being produced using copper, zinc, titanium, magnesium, gold, alginate and silver.
The nanoparticles (NPs) differ from various dimensions, to shapes and sizes apart from their material. It
be spherical, cylindrical, tubular, conical, hollow core, spiral, flat, etc. or irregular and differ from 1 nm
to 100 nm in size. The surface can be a uniform or irregular with surface variations. Some nanoparticles
are crystalline or amorphous with single or multi crystal solids either loose or agglomerated. It can be
either a zero dimensional where the length, breadth and height is fixed at a single point for example nano
dots, one dimensional where it can possess only one parameter for example graphene, two dimensional
where it has length and breadth for example carbon nanotubes or three dimensional where it has all the
parameters such as length, breadth and height for example gold nanoparticles. Numerous synthesis
methods are either being developed or improved to enhance the properties and reduce the production
costs. Some methods are modified to achieve process specific nanoparticles to increase their optical,
mechanical, physical and chemical properties . A vast development in the instrumentation has led to an
improved nanoparticle characterisation and subsequent application.
NPs are being used for diverse purposes, from medical treatments, using in various branches of industry
production such as solar and oxide fuel batteries for energy storage, to wide incorporation into diverse
materials of everyday use such as cosmetics or clothes. It offers a Ialth of tools to diagnose and treat
cancer—new imaging agents, multifunctional, targeted devices capable of bypassing biological barriers
to deliver therapeutic agents directly to cells and tissues involved in cancer growth and metastasis,
monitor predictive molecular changes allowing preventive action against precancerous cells, and
minimizing costs and side effects.
Personalized medicine could become a reality in cancer patient management.
The reason why these Engineered nanoparticles (NPs) are attractive for medical purposes is based on
their important and unique features, such as their surface to mass ratio that is much larger than that of
other particles, their quantum properties and their ability to adsorb and carry other compounds. NPs have
a relatively large (functional) surface which is able to bind, adsorb and carry other compounds such as
drugs, probes and proteins. The composition of the engineered nanoparticles may vary. Source materials
may be of biological origin like phospholipids, lipids, lactic acid, dextran, chitosan, or have more
“chemical” characteristics like various polymers, carbon, silica, and metals. The interaction with cells for
some of the biological components like phospholipids will be quite different compared to the non
biological components such as metals like iron or cadmium. The primary goals for research of nano-bio-
technologies in drug delivery include: More specific drug targeting and delivery, reduction in
toxicity while maintaining therapeutic effects,greater safety and biocompatibility and faster
development of new safe medicines.
Copper NPs may cause fluorescence quenching, dye aggregation, dye deaggregation, and fluorescence
enhancement. This property may be used for biosensing and biolabeling (Mandal and De 2015).
Copper-based drugs are widely used to destabilize tumors and cancer cells.
Polymer fillers are also broadly used for altering the permeability of polymer films. Orthopedic
surgery has been the first to profit from nanoparticulate biomaterials. Here,mainly inert or biologically
tolerated materials Ire used for improving healing, implant adhesion and tissue response. Gold
nanoparticles combine mobility, strong colouration and the possibility for attachment of biomolecules,
these noble metal particles are being used in diagnostic tools, e.g.pregnancy tests that can be read
optically.
Nanotechnology also takes part in the production of nanofertilizers for increasing the efficacy and
bioavailability of such new fertilizers as Ill as decreasing the loss of these materials to the surrounding
environment .The application of nanotechnology in the agri-food sector is one of the fastest-growing
fields in nano-research. The application of nanoagrochemicals seems crucial for promoting the modern
type of agriculture. Here application of nanotechnology include: 1) nanoformulations of agrochemicals
for applying pesticides and fertilizers for crop improvement;
2) the application of nanosensors/nanobiosensors in crop protection for the identification of diseases and
residues of agrochemicals; 3) nanodevices for the genetic manipulation of plants;
4) plant disease diagnostics; 5) animal health, animal breeding, poultry production; and 6) postharvest
management. Nanopesticides offer a way to both control delivery of pesticides and achieve greater
effects with a specific chemical dose.
(2) Review of Literature
(2.1) Nanoparticles
Copper: Copper nanoparticles have prospective applications in optics, electronics, and medicine and in
manufacturing of lubrications, nanofluids, conductive films, and antimicrobial agents. The preference of
copper nanoparticles compared to silver is due to the lower cost of copper than silver, the physical and
chemical stability, and ease of mixing with. Smaller nanoparticles offer higher activity but may result in
cluster formation causing a decrease in essential properties.
Metal nanoparticles possess fascinating ultraviolet–visible sensitivity, electrical, catalytic, thermal, and
antibacterial properties due to the reasons: quantum effects and large surface-to- volume ratio. A large
number of atoms are present on the surface due to smaller particle size. The surface area-to-volume
ratio of particles varies by depending on the shape and size of nanoparticles, including the ultraviolet–
visible sensitivity and conductivity. The characteristic properties including the electronic energy levels,
electron affinity, electronic transitions, magnetic properties, phase transition temperature, melting point,
and affinity to polymers, biological and organic molecules are also modulated by the change in surface
area.
Quantum effects are due to the combination of quantum size and Coulomb charging effects that impart
the charge to nanoparticles. When the Coulomb charge effect is coupled with the quantum size, a range
of fascinating properties are obtained that are not observed for the same bulk material. Quantum effects
are prominent in spherical particles and in particles with sharp edges. Due to these effects and their size-
dependent nature, nanoparticles are used in catalysis, sensing, and imaging.
Silver: Silver nanoparticles have proved to be most effective because of it’s good
antimicrobial efficacy against bacteria, viruses and other eukaryotic micro-organisms. They
are undoubtedly the most widely used nanomaterials among all, thereby being used as
antimicrobial agents, in textile industries, for water treatment, sunscreen lotions etc. Studies
have already reported the successful biosynthesis of silver nanoparticles by plants such as
Azadirachta indica , Capsicum annuum and Carica papaya .
Gold: Gold nanoparticles (AuNPs) are used in immunochemical studies for identification of
protein interactions. They are used as lab tracer in DNA fingerprinting
to detect presence of DNA in a sample. They are also used for detection of aminoglycoside
antibiotics like streptomycin, gentamycin and neomycin. Gold nanorods are being used to
detect cancer stem cells, beneficial for cancer diagnosis and for identification of different
classes of bacteria.
Alloy: Alloy nanoparticles exhibit structural properties that are different from their bulk
samples. Since Ag has the highest electrical conductivity among metal fillers and, unlike many
other metals, their oxides have relatively better conductivity, Ag flakes are most widely used.
Bimetallic alloy nanoparticles properties are influenced by both metals and show more
advantages over ordinary metallic NPs.
Magnetic: Magnetic nanoparticles like Fe3O4 (magnetite) and Fe2O3 (maghemite) are
known to be biocompatible. They have been actively investigated for targeted cancer
treatment (magnetic hyperthermia), stem cell sorting and manipulation, guided drug delivery,
gene therapy, DNA analysis, and magnetic resonance imaging (MRI)2
Fullerenes
Fullerenes are an allotropic modification of carbon, often termed as a molecular form of carbon, or
carbon molecules. The fullerene family includes a number of atomic C n clusters (n > 20), composed of
carbon atoms on a spherical surface. Carbon atoms are usually located on the
surface of the sphere at the vertices of pentagons and hexagons. In fullerenes, carbon atoms are usually
present in the sp2-hybrid form and linked together by covalent bonds. Fullerene C60 is the most common
and best-investigated fullerene. The spherical molecule is highly symmetric and consists of 60 carbon
atoms, located at the vertices of tInty hexagons and tIlve pentagons (Fig. 2c). The diameter of fullerene
C60 is 0.7 nm.
Among other carbon-based nanomaterials, CNTs are one of the carbon allotropes with exceptional
properties suitable for technical applications. They are characterized by cylindrical structures with a
diameter of several nanometers, consisting of rolled graphene sheets (Fig. 2d). Carbon nanotubes may
vary in length, diameter, chirality (symmetry of the rolled graphite sheet) and the number of layers.
According to their structure, CNTs may be classified into two main groups: single-walled nanotubes
(SWCNTs) and multi-walled nanotubes (MWCNTs).The structure of CNTs leads to exceptional
properties with a unique combination of rigidity, strength and elasticity compared with other fibrous
materials. CNTs show high thermal and electrical conductivity compared to other conductive materials.
Electrical properties of SWCNTs depend on their chirality or hexagon orientation with respect to the tube
axis. Accordingly, SWCNTs are classified into three sub-classes: (i) armchair (electrical conductivity >
copper), (ii) zigzag (semi- conductive properties) and (iii) chiral (semi-conductive properties) (Fig. 2e).
By contrast, MWCNTs consisting of multiple carbon layers, frequently with variable chirality, can exhibit
extraordinary mechanical properties instead of outstanding electrical characteristics.
Graphene
Graphene is a two-dimensional allotropic form of carbon, formed by single layers of carbon atoms
(Fig. 2f). In graphene, carbon atoms exhibit sp2-hybridization connected by σ- and π- bonds in a two-
dimensional hexagonal crystal lattice with a distance of 0.142 nm betIen neighboring atoms of carbon
hexagons. It also represents a structural element of some other carbon allotropes, such as graphite,
carbon nanotubes and fullerenes. It has many unique physical properties, such as extremely high
mechanical rigidity and a high thermal stability. Also the electric properties of this carbon allotrope
are fundamentally different from the properties of three-dimensional materials.
Fig 2- Structure of a carbon atom and of carbon-based nanoparticles. a Electronic configuration of a
carbon atom before and after promotion of one electron; b schematic representation of a carbon atom
structure with two electron orbitals around the nucleus and six electrons distributed on them; c structure
of a fullerene C60; d structure of a single-walled nanotube; e different types of single-walled nanotubes:
armchair, zig-zag and chiral; f structure of a graphene
sheet; g structure of an oxidized single-walled nanotube
Chitosan
It is a biodegradable, biocompatible polymer regarded as safe for human dietary use and approved for
wound dressing applications. It has been used as a carrier in polymeric nanoparticles for drug delivery
through various routes of administration. It has chemical functional groups that can be modified to
achieve specific goals, making it a polymer with a tremendous range of potential applications.
Nanoparticles (NP) prepared with chitosan and chitosan derivatives typically possess a positive surface
charge and mucoadhesive properties such that can adhere to mucus membranes and release the drug
payload in a sustained release manner. Chitosan-based NP have various applications in non-parenteral
drug delivery for the treatment of cancer, gastrointestinal diseases, pulmonary diseases, drug delivery to
the brain and ocular infections which will be exemplified in this review. Chitosan shows low toxicity both
in vitro and some in vivo models.
Chitosan is the most important derivative of chitin, produced by removing the acetate moiety from
chitin as shown below
It is derived from crustacean shells such as those from prawns or crabs, as well as from the cell walls of
fungi. It is a naturally occurring polysaccharide, cationic, highly basic, mucoadhesive biocompatible
polymer and approved by the U.S. FDA for tissue engineering and drug delivery. Chitosan acts a
penetration enhancer by opening the tight junctions of the epithelium. It facilitates both paracellular and
transcellular transport of drugs.
The chitosan backbone can be modified to alter properties such as solubility, mucoadhesion and stability.
Some of the commonly used techniques for preparing chitosan polymers are: blending, graft co-
polymerization and curing. Blending involves the simple mixing of two or more polymers. Graft co-
polymerization involves the covalent bonding of polymers, while curing converts the polymers into a
solidified mass by formation of three-dimensional bonds within the polymer mass by means of thermal,
electrochemical or ultraviolet radiation processing methods.
(4) Composite-based nanomaterials: The composite nanomaterials are any combination of metal-
based, metal oxide-based, carbon-based, and/or organic-based nanomaterials, and these nanomaterials
have complicated structures like a metal-organic framework. Nanocomposites are a new generation of
novel materials, which are formed by mixing one or more dissimilar materials at the nanoscale in order to
control and develop new and improved structures as well as properties .The term nanocomposite
encompasses a wide range of materials right from
three-dimensional metal matrix composites, two-dimensional lamellar composites, and nanowires of
single dimension to zero-dimensional core shells representing many variations of nanomixed and layered
materials. The properties of nanocomposites depend not only upon the
individual components used, but also upon the morphology and the interface
Enhanced properties such as improved friction and abrasion resistance, fouling resistance,
super hydrophobicity, super hydrophilicity, thermal energy transport, electronic and ionic
transport, and liquid transport displayed by nanocomposites compared to individual materials make
them attractive for a wide range of engineering applications.
Cu nanoparticles were prepared by dissolving 3 g of copper sulphate in 100 ml 5% acetic acid (v/v).
The mixture was stirred using a magnetic stirrer for 2 h.
Then addition of 2 M NaOH was done dropwise until the whole copper sulphate present in the solution
got precipitated into copper hydroxide.
After settling, the sample was centrifuged at 10,000 rpm for 15 mins.The sample was then
Ultrasonicated for 15 mins and then again centrifuged at 10,000 rpm for 15 mins. The sample was
washed and the supernatant was discarded. The pellets were left to dry. The dried pellets were then
crushed using a mortar and pestle to form a fine powder. The sample was further examined by X-Ray
Diffraction.
Fig 5- Copper sulphate mixed with Acetic Acid for the formation of Cu NPs
Chitin nanoparticles were prepared by dissolving chitin flakes (1 g) in 100 ml 5% acetic acid (v/v).
The mixture was stirred using a magnetic stirrer for 2 h.
After settling, the sample was centrifuged at 10,000 rpm for 15 mins.
The sample was then Ultrasonicated for 15 mins and then again centrifuged at 10,000 rpm for 15 mins.
The sample was washed and the supernatant was discarded. The
pellets were left to dry.
The dried pellets were then crushed using a mortar and pestle to form a fine powder. The sample was
further examined by X-Ray Diffraction.
Copper-Chitin nanoparticles were prepared by dissolving chitin flakes (1 g) in 100 ml 5% acetic acid
(v/v).
The mixture was stirred using a magnetic stirrer for 2 h.
Then 3 g of copper sulphate was added to the chitosan solution followed by the
addition of 2 M NaOH dropwise until the whole copper sulphate present in the solution got
precipitated into copper hydroxide.
This also helps in the coagulation of chitin and copper gets coated by chitin. After
settling, the sample was centrifuged at 10,000 rpm for 15 mins.
The sample was then Ultrasonicated for 15 mins and then again centrifuged at 10,000 rpm for 15 mins.
The sample was washed and the supernatant was discarded. The
pellets were left to dry.
The dried pellets were then crushed using a mortar and pestle to form a fine powder. The sample was
further examined by X-Ray Diffraction.
Fig 6 - Copper sulphate mixed with Acetic Acid and chitin flakes
Copper-Chitin nanopesticide was prepared by dissolving chitin flakes (1 g) in 100 ml 5% acetic acid
(v/v).
The mixture was stirred using a magnetic stirrer for 2 h.
Then 3 g of copper sulphate was added to the chitosan solution followed by the
addition of 2 M NaOH dropwise until the whole copper sulphate present in the solution got precipitated
into copper hydroxide.
Then 1ml of a pesticide was added to the sample and shaked well. After
settling, the sample was centrifuged at 10,000 rpm for 15 mins.
The sample was then Ultrasonicated for 15 mins and then again centrifuged at 10,000 rpm for 15 mins.
The sample was washed and the supernatant was discarded. The
pellets were left to dry.
The dried pellets were then crushed using a mortar and pestle to form a fine powder. The sample
was further examined by X-Ray Diffraction.
Fig 7 – Ultrasonication of the Nanopesticide sample
(4) Result and Discussion
After the addition of NaOH to the samples the precipitate formation starts which can be detected by the
change in the colour of the sample as shown in Fig 8.
The pellets can be observed in the sample after centrifugation as shown in Fig 10
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15.7986 2.21 0.3840 5.60493 6.11
16.9940 2.22 0.5760 5.21327 6.15
19.0650 8.08 0.6720 4.65136 22.35
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35.8748 10.50 0.6720 2.50115 29.05
38.4198 19.95 0.3840 2.34112 55.20
42.1673 1.47 0.3840 2.14132 4.08
42.9626 1.83 0.3840 2.10351 5.06
44.6972 36.15 0.5760 2.02582 100.00
48.8834 4.40 0.7680 1.86167 12.16
52.7605 4.63 0.5760 1.73363 12.80
56.1659 1.87 0.4800 1.63632 5.16
57.3610 1.35 1.5360 1.60504 3.73
61.4893 3.33 0.5760 1.50681 9.21
65.1409 3.75 0.5760 1.43089 10.37
66.6596 2.55 0.6720 1.40193 7.05
68.2878 3.44 0.5760 1.37241 9.52
73.1477 0.68 3.0720 1.29276 1.87
74.2196 1.56 0.3840 1.27672 4.32
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Comment Configuration=KU 18/05/10, Owner=User-1, Creation date=5/18/2010
11:42:07 AM
Goniometer=PW3050/60 (Theta/Theta); Minimum step size
2Theta:0.001; Minimum step size Omega:0.001
Sample stage=PW3071/xx Bracket
Diffractometer system=XPERT-PRO
Measurement program=Powder BB Scan, Owner=User-1, Creation
date=5/19/2010 12:37:38 PM
Measurement Date / Time 12/21/2022 10:54:52 AM
Operator Kurukshetra Universi
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16.9940 2.22 0.5760 5.21327 6.15
19.0650 8.08 0.6720 4.65136 22.35
20.4875 3.70 0.3840 4.33150 10.23
23.5965 3.63 0.7680 3.76736 10.05
24.0332 3.87 0.3840 3.69989 10.69
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29.5504 1.29 0.5760 3.02046 3.56
32.4394 1.72 0.5760 2.75775 4.75
34.1383 3.51 0.7680 2.62430 9.72
35.8748 10.50 0.6720 2.50115 29.05
38.4198 19.95 0.3840 2.34112 55.20
42.1673 1.47 0.3840 2.14132 4.08
42.9626 1.83 0.3840 2.10351 5.06
44.6972 36.15 0.5760 2.02582 100.00
48.8834 4.40 0.7680 1.86167 12.16
52.7605 4.63 0.5760 1.73363 12.80
56.1659 1.87 0.4800 1.63632 5.16
57.3610 1.35 1.5360 1.60504 3.73
61.4893 3.33 0.5760 1.50681 9.21
65.1409 3.75 0.5760 1.43089 10.37
66.6596 2.55 0.6720 1.40193 7.05
68.2878 3.44 0.5760 1.37241 9.52
73.1477 0.68 3.0720 1.29276 1.87
74.2196 1.56 0.3840 1.27672 4.32
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- Modification editor = "Kurukshetra Universi"
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- Intensity ratio = "0.50"
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- Modification editor = "Kurukshetra Universi"
Smooth:
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- Method = "Minimum 2nd derivative"
- Modification time = "8/18/2016 12:00:03 PM"
- Modification editor = "Kurukshetra Universi"
Measurement Conditions: (Sample 3)
Dataset Name 3
File name C:\X'Pert Data\XRD\out side\kuk\uiet\aarzoo rana\211222\3.xrdml
Comment Configuration=KU 18/05/10, Owner=User-1, Creation date=5/18/2010
11:42:07 AM
Goniometer=PW3050/60 (Theta/Theta); Minimum step size
2Theta:0.001; Minimum step size Omega:0.001
Sample stage=PW3071/xx Bracket
Diffractometer system=XPERT-PRO
Measurement program=Powder BB Scan, Owner=User-1, Creation
date=5/19/2010 12:37:38 PM
Measurement Date / Time 12/21/2022 11:14:35 AM
Operator Kurukshetra Universi
Raw Data Origin XRD measurement (*.XRDML)
Scan Axis Gonio
Start Position [°2Th.] 10.0100
End Position [°2Th.] 79.9900
Step Size [°2Th.] 0.0200
Scan Step Time [s] 0.1000
Scan Type Continuous
Offset [°2Th.] 0.0000
Divergence Slit Type Fixed
Divergence Slit Size [°] 0.9570
Specimen Length [mm] 10.00
Receiving Slit Size [mm] 3.0300
Measurement Temperature [°C] 25.00
Anode Material Cu
K-Alpha1 [Å] 1.54060
Generator Settings 40 mA, 45 kV
Diffractometer Type 0000000011059335
Diffractometer Number 0
Goniometer Radius [mm] 240.00
Dist. Focus-Diverg. Slit [mm] 91.00
Incident Beam Monochromator No
Spinning No
Main Graphics, Analyze View: (Bookmark 2)
Counts
3
30
20
10
20 30 40 50 60 70
Pos. [°2Th.] Height [cts] FWHM [°2Th.] d-spacing [Å] Rel. Int. [%]
13.2617 1.95 0.7680 6.67085 6.88
14.8270 1.30 0.9600 5.96994 4.60
15.9527 1.19 0.5760 5.55112 4.21
21.5844 1.39 1.9200 4.11380 4.92
29.3726 1.47 0.5760 3.03833 5.21
32.3767 0.44 1.7280 2.76295 1.57
35.1124 8.55 1.1520 2.55369 30.21
38.2688 17.19 0.6720 2.35001 60.77
44.6555 28.29 0.5760 2.02762 100.00
48.2629 5.41 0.4800 1.88415 19.12
50.0304 1.49 0.3840 1.82165 5.27
51.9290 0.97 0.3840 1.75942 3.42
53.5538 2.07 0.4800 1.70981 7.32
56.7889 1.99 0.3840 1.61984 7.02
60.9930 2.70 1.5360 1.51787 9.54
63.0462 1.26 0.3840 1.47329 4.46
65.1467 4.94 0.5760 1.43077 17.45
67.4111 5.87 0.7680 1.38811 20.74
70.1290 0.84 0.3840 1.34082 2.97
72.3434 2.58 1.1520 1.30513 9.11
Insert Measurement:
- File name = "3.xrdml"
- Modification time = "12/21/2022 2:27:01 PM"
- Modification editor = "Kurukshetra Universi"
Default properties:
- Measurement step axis = "None"
- Internal wavelengths used from anode material: Copper (Cu)
- Original K-Alpha1 wavelength = "1.54060"
- Used K-Alpha1 wavelength = "1.54060"
- Original K-Alpha2 wavelength = "1.54443"
- Used K-Alpha2 wavelength = "1.54443"
- Original K-Beta wavelength = "1.39225"
- Used K-Beta wavelength = "1.39225"
- Dist. focus to div. slit = "91.00000"
- Irradiated length = "10.00000"
- Spinner used = "No"
- Linear detector mode = "None"
- Length linear detector = "2"
- Step axis value = "0.00000"
- Offset = "0.00000"
- Sample length = "10.00000"
- Modification time = "12/21/2022 2:27:01 PM"
- Modification editor = "Kurukshetra Universi"
Subtract Background:
- Correction method = "Automatic"
- Bending factor = "8"
- Use smoothed input data = "Yes"
- Granularity = "51"
- Add to net scan = "Nothing"
- Modification time = "5/12/2014 11:34:02 AM"
- Modification editor = "Kurukshetra Universi"
Strip K-Alpha2:
- Method = "Rachinger"
- Intensity ratio = "0.50"
- Delta wavelength ratio = "0.000000"
- Modification time = "5/19/2010 11:25:33 AM"
- Modification editor = "Kurukshetra Universi"
Smooth:
- Type of smoothing = "Polynomial"
- Polynomial type = "Cubic"
- Convolution range = "25"
- Modification time = "3/21/2016 4:21:48 PM"
- Modification editor = "Kurukshetra Universi"
Search Peaks:
- Minimum significance = "0.50"
- Minimum tip width = "0.25"
- Maximum tip width = "7.00"
- Peak base width = "10.00"
- Method = "Minimum 2nd derivative"
- Modification time = "8/18/2016 12:00:03 PM"
- Modification editor = "Kurukshetra Universi"
Measurement Conditions: (Sample 4)
Dataset Name 4
File name C:\X'Pert Data\XRD\out side\kuk\uiet\aarzoo rana\211222\4.xrdml
Comment Configuration=KU 18/05/10, Owner=User-1, Creation date=5/18/2010
11:42:07 AM
Goniometer=PW3050/60 (Theta/Theta); Minimum step size
2Theta:0.001; Minimum step size Omega:0.001
Sample stage=PW3071/xx Bracket
Diffractometer system=XPERT-PRO
Measurement program=Powder BB Scan, Owner=User-1, Creation
date=5/19/2010 12:37:38 PM
Measurement Date / Time 12/21/2022 11:26:22 AM
Operator Kurukshetra Universi
Raw Data Origin XRD measurement (*.XRDML)
Scan Axis Gonio
Start Position [°2Th.] 10.0100
End Position [°2Th.] 79.9900
Step Size [°2Th.] 0.0200
Scan Step Time [s] 0.1000
Scan Type Continuous
Offset [°2Th.] 0.0000
Divergence Slit Type Fixed
Divergence Slit Size [°] 0.9570
Specimen Length [mm] 10.00
Receiving Slit Size [mm] 3.0300
Measurement Temperature [°C] 25.00
Anode Material Cu
K-Alpha1 [Å] 1.54060
Generator Settings 40 mA, 45 kV
Diffractometer Type 0000000011059335
Diffractometer Number 0
Goniometer Radius [mm] 240.00
Dist. Focus-Diverg. Slit [mm] 91.00
Incident Beam Monochromator No
Spinning No
Main Graphics, Analyze View: (Bookmark 2)
Counts
4
40
20
20 30 40 50 60 70
Pos. [°2Th.] Height [cts] FWHM [°2Th.] d-spacing [Å] Rel. Int. [%]
11.6196 4.88 0.3840 7.60967 10.20
13.2464 1.56 0.9600 6.67854 3.25
17.0963 10.86 0.3840 5.18230 22.71
19.0444 35.28 0.5760 4.65636 73.73
21.1722 10.48 0.7680 4.19295 21.89
22.6816 9.17 0.7680 3.91722 19.16
23.8126 3.30 0.7680 3.73366 6.90
25.1101 4.08 0.5760 3.54359 8.53
28.1530 2.73 0.3840 3.16712 5.71
29.6968 5.60 0.9600 3.00590 11.71
31.0207 1.16 0.5760 2.88057 2.42
32.5006 2.62 0.5760 2.75270 5.48
33.7857 5.01 0.4800 2.65087 10.47
35.6248 6.01 0.3840 2.51813 12.57
36.7918 3.90 0.4800 2.44089 8.14
38.4311 12.67 0.5760 2.34046 26.48
40.7169 1.78 0.7680 2.21419 3.72
44.6671 47.85 0.5760 2.02711 100.00
45.4112 0.99 0.3840 1.99561 2.07
46.5982 1.78 0.5760 1.94751 3.71
48.1083 2.49 0.6720 1.88984 5.21
51.0825 2.10 1.1520 1.78657 4.39
52.4366 2.10 0.3840 1.74358 4.38
56.0586 1.61 0.5760 1.63920 3.36
60.6379 1.79 0.3840 1.52591 3.74
65.0886 4.88 0.3840 1.43191 10.20
72.8490 5.97 0.7680 1.29732 12.47
74.4215 1.75 0.3840 1.27375 3.66
78.2063 4.58 0.3840 1.22130 9.57
Insert Measurement:
- File name = "4.xrdml"
- Modification time = "12/21/2022 2:27:33 PM"
- Modification editor = "Kurukshetra Universi"
Default properties:
- Measurement step axis = "None"
- Internal wavelengths used from anode material: Copper (Cu)
- Original K-Alpha1 wavelength = "1.54060"
- Used K-Alpha1 wavelength = "1.54060"
- Original K-Alpha2 wavelength = "1.54443"
- Used K-Alpha2 wavelength = "1.54443"
- Original K-Beta wavelength = "1.39225"
- Used K-Beta wavelength = "1.39225"
- Dist. focus to div. slit = "91.00000"
- Irradiated length = "10.00000"
- Spinner used = "No"
- Linear detector mode = "None"
- Length linear detector = "2"
- Step axis value = "0.00000"
- Offset = "0.00000"
- Sample length = "10.00000"
- Modification time = "12/21/2022 2:27:33 PM"
- Modification editor = "Kurukshetra Universi"
Subtract Background:
- Correction method = "Automatic"
- Bending factor = "8"
- Use smoothed input data = "Yes"
- Granularity = "51"
- Add to net scan = "Nothing"
- Modification time = "5/12/2014 11:34:02 AM"
- Modification editor = "Kurukshetra Universi"
Strip K-Alpha2:
- Method = "Rachinger"
- Intensity ratio = "0.50"
- Delta wavelength ratio = "0.000000"
- Modification time = "5/19/2010 11:25:33 AM"
- Modification editor = "Kurukshetra Universi"
Smooth:
- Type of smoothing = "Polynomial"
- Polynomial type = "Cubic"
- Convolution range = "25"
- Modification time = "3/21/2016 4:21:48 PM"
- Modification editor = "Kurukshetra Universi"
Search Peaks:
- Minimum significance = "0.50"
- Minimum tip width = "0.25"
- Maximum tip width = "7.00"
- Peak base width = "10.00"
- Method = "Minimum 2nd derivative"
- Modification time = "8/18/2016 12:00:03 PM"
- Modification editor = "Kurukshetra Universi"
Measurement Conditions: (Sample 5)
Dataset Name 5
File name C:\X'Pert Data\XRD\out side\kuk\uiet\aarzoo rana\211222\5.xrdml
Comment Configuration=KU 18/05/10, Owner=User-1, Creation date=5/18/2010
11:42:07 AM
Goniometer=PW3050/60 (Theta/Theta); Minimum step size
2Theta:0.001; Minimum step size Omega:0.001
Sample stage=PW3071/xx Bracket
Diffractometer system=XPERT-PRO
Measurement program=Powder BB Scan, Owner=User-1, Creation
date=5/19/2010 12:37:38 PM
Measurement Date / Time 12/21/2022 11:38:30 AM
Operator Kurukshetra Universi
Raw Data Origin XRD measurement (*.XRDML)
Scan Axis Gonio
Start Position [°2Th.] 10.0100
End Position [°2Th.] 79.9900
Step Size [°2Th.] 0.0200
Scan Step Time [s] 0.1000
Scan Type Continuous
Offset [°2Th.] 0.0000
Divergence Slit Type Fixed
Divergence Slit Size [°] 0.9570
Specimen Length [mm] 10.00
Receiving Slit Size [mm] 3.0300
Measurement Temperature [°C] 25.00
Anode Material Cu
K-Alpha1 [Å] 1.54060
Generator Settings 40 mA, 45 kV
Diffractometer Type 0000000011059335
Diffractometer Number 0
Goniometer Radius [mm] 240.00
Dist. Focus-Diverg. Slit [mm] 91.00
Incident Beam Monochromator No
Spinning No
Pos. [°2Th.] Height [cts] FWHM [°2Th.] d-spacing [Å] Rel. Int. [%]
12.6181 1.32 0.3840 7.00966 3.49
19.2716 35.95 1.0560 4.60195 95.18
20.9220 11.45 0.7680 4.24252 30.31
23.5811 4.57 1.5360 3.76978 12.10
26.2159 10.57 0.4800 3.39658 27.99
29.7153 4.19 1.1520 3.00408 11.10
31.8511 1.35 0.5760 2.80733 3.58
34.5349 0.48 0.3840 2.59507 1.26
35.5720 1.48 0.4800 2.52174 3.93
36.8764 1.08 0.5760 2.43548 2.87
38.3955 5.02 0.4800 2.34255 13.28
44.6748 37.78 0.5760 2.02678 100.00
51.4359 2.08 0.3840 1.77512 5.51
52.3499 1.68 0.3840 1.74626 4.45
56.5620 2.85 0.3840 1.62580 7.53
57.8100 2.19 1.5360 1.59364 5.79
60.3839 2.54 0.3840 1.53172 6.72
62.3018 0.97 1.1520 1.48909 2.58
64.9432 1.92 0.5760 1.43477 5.09
65.7264 1.94 0.3840 1.41955 5.12
69.9618 0.80 0.7680 1.34361 2.12
72.8548 14.04 0.6720 1.29723 37.16
Insert Measurement:
- File name = "5.xrdml"
- Modification time = "12/21/2022 2:28:04 PM"
- Modification editor = "Kurukshetra Universi"
Default properties:
- Measurement step axis = "None"
- Internal wavelengths used from anode material: Copper (Cu)
- Original K-Alpha1 wavelength = "1.54060"
- Used K-Alpha1 wavelength = "1.54060"
- Original K-Alpha2 wavelength = "1.54443"
- Used K-Alpha2 wavelength = "1.54443"
- Original K-Beta wavelength = "1.39225"
- Used K-Beta wavelength = "1.39225"
- Dist. focus to div. slit = "91.00000"
- Irradiated length = "10.00000"
- Spinner used = "No"
- Linear detector mode = "None"
- Length linear detector = "2"
- Step axis value = "0.00000"
- Offset = "0.00000"
- Sample length = "10.00000"
- Modification time = "12/21/2022 2:28:04 PM"
- Modification editor = "Kurukshetra Universi"
Subtract Background:
- Correction method = "Automatic"
- Bending factor = "8"
- Use smoothed input data = "Yes"
- Granularity = "51"
- Add to net scan = "Nothing"
- Modification time = "5/12/2014 11:34:02 AM"
- Modification editor = "Kurukshetra Universi"
Strip K-Alpha2:
- Method = "Rachinger"
- Intensity ratio = "0.50"
- Delta wavelength ratio = "0.000000"
- Modification time = "5/19/2010 11:25:33 AM"
- Modification editor = "Kurukshetra Universi"
Smooth:
- Type of smoothing = "Polynomial"
- Polynomial type = "Cubic"
- Convolution range = "25"
- Modification time = "3/21/2016 4:21:48 PM"
- Modification editor = "Kurukshetra Universi"
Search Peaks:
- Minimum significance = "0.50"
- Minimum tip width = "0.25"
- Maximum tip width = "7.00"
- Peak base width = "10.00"
- Method = "Minimum 2nd derivative"
- Modification time = "8/18/2016 12:00:03 PM"
- Modification editor = "Kurukshetra Universi"
(5) CONCLUSION
A novel copper chitosan nanocomposite has been prepared and characterized by various
instrumental techniques. The particle size ranged from 700 to 750 nm. Adsorbent– adsorbate
systems were modeled by both Langmuir and Freundlich isotherms. The maximum adsorption
capacity was found to be 322.6±3.5 mg g-1 of the adsorbent. Using XRD studies, a suitable
mechanism for the adsorption has been proposed.
.
(6) References