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Assist. Prof. Dr. Ahlam Hussien Al Musawi
Assist. Prof. Dr. Natiq Abdullah Ali
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Russia - Biology
Prof. Dr. Marie M. El-Ajaily
Libya - Banghazi Uni. - Chemists
Prof. Dr. Omar Shhab Hamad Al-Obaidi Prof. Dr. Nabil Mohie El-Deen Abdel-Hamid Prof. Dr. Mahmoud Ahmed Souror
Prof. Dr. Taghreed Hashim Al-Noor Prof. Dr. Mohammed Saleh Mahdi
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Dr. Zaid Muslim
Dr. Nagham Thamir Ali
Iraq - Chemists
Egypt - Kafr Al-Sheikh Uni. - Pharmacy Lebanon - Lebanon Uni.
Iraq - President of the A. Ch.S. Chapter of Iraq - Chemists Iraq - Laser Eng. Iraq - Laser Eng.
Iraq - Al-Kut Univ. College - Pharmacy Iraq - Laser Phys.
Iraq - Al-Kut Univ. College
Iraq - Al-Kut Univ. College - Dentistry U.K. - Derm Uni. - Physics
Iraq- Al-Mustansiriya Uni. – Mathematical Statistics Iraq - Al-Kut Univ. College - Laser Phys Iraq - Al-Kut Univ. College - Laser Phys Iraq - Al-Kut Univ. College
Iraq - Ministry of Science & Technology - Laser Phys
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مجلة كلية الكوت الجامعة
Vol. 4
Issue 2
2019
4th Year
Papers in English
No: Title and the Name of Researchers 1
Pages
Design and Construction of a Laser Pressure Fiber Sensor
1-8
Rabi N. Al- Waali, Dr. Talib Zeedan Taban and Esam Abbas Khudhair 2
Study the Optical and Structural Properties SnO2 Films Grown by (APCVD)
9-17
Nagham T. Ali and Talib Zeedan T. Al-Mosawi 3
Comparison of Antibacterial Effect of Biosynthesis Nanoparticles with Chemically Synthesis Nanoparticles in Vitro
18-28
Meraim A. Kazaal 4
Concentrations and [pH] Effects on Spectral Shifts of C6H6 and CCl4 Compounds
Mohammed S. Mahde, M.R. Mohammad and Haneen Muthanna Awad
VI
29-37
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مجلة كلية الكوت الجامعة
Vol. 4
Issue 2
2019
4th Year
Design and Construction of a Laser Pressure Fiber Sensor Rabi N. Al - Waali*, Dr. Talib Zeedan Taban** and Esam Abbas Khudhair*** Al-kut University College –Iraq *rabi942@yahoo.com **talibmosawi@gmail.com ***esam.abas90@gmail.com
Abstract This paper investigates optical fiber pressure sensor which based on periodic microbending losses phenomenon. Deform cells made of aluminum material of dimension (30˟100) mm are designed and constructed with periodic microbends of spatial periodicity of 8 mm. Distance separation between two deform plates is 6mm and 8 mm through which the optical fiber PCS380 passes. The light emitting diode of 650nm is used as a source. Pressure force has been applied on the deform cells by using various masses (0.5-5) Kg. The mechanical instrument which used to apply pressure force on deform cells. The value of mass appears on an analogous gauge. The output power and intensity spectrum are recorded at different pressure forces. الخالصة الب سسسخيل ظالر ما نصن ءغهخا اايحرغياط ال غييخظيلن ان ن يل اايحرغي
ان هذا البحث يدرس متحسسسسسسسسغط اللسس ا لصليغ
م م ظالذي ي ثل ال سسغةل بيا لل ايحرغي ظخنخن مم8 ( م م ظان البعد الدظري لصيحرغي هع30x100) م سرعةل ما مغةا اال ريع ااط أبعغة ن ان اللسعي ال غر هع وسعي الدايعة البغةث ل لسعي ظب عن معpcs380
م م مع ليف ب سخي ما يع6 م م ظن يل8 اسستع غن ن يل
( ل من ظمم مصحظل الت ييخ ة القدرا ظالشسسسدا0.5-5) لعا ة ب الع يل بغسسسستع غن لتل معت ل
سسسدر وسسسعط ظسس س
يغيعمتخ ل650
العغر تيا مع مديغط معت ل ما لعى الل ان
1
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Vol. 4 Issue 2 2019 4th Year
themselves useful for detecting environmental
Introduction Optical fiber sensors are used to measure
changes. Many different mechanical elements
temperature, pressure, chemical species, strain,
have been developed to perform the sensing, each
moisture, force, displacement, acceleration, etc.
with
[1-5]. Optical fiber, microbend sensor, is based on
application.
attributes
suitable
for
a
particular
The sensor structure can be simple and
the control and analysis of couplings and leakage of modes propagating in a deformed microbend
regular
periodical
optical
microlending
is
optical fiber [6-10]. Sensing of losses in deformed
generated to create microbendings in small portion
fiber is done by output power measurements.
of the optical fiber which is placed between a pair of deformation plates as shown in Fig. (1).
Optical fiber pressure sensors are widely applied due to their advantages of low cost, light
By microbendings the fiber is bent to
weight, flexible structure design and not being
critical angle and some modes escape from the
affected by electromagnetic field.
core to the cladding. It leads to changes in the
According to sensing principle, optical
intensity of back-scattered radiation from the place
fiber pressure sensors can be divided into
of effect. The plates in response of change is of
intensity-based,
polarization,
physical quantity ΔE acts as a force ΔF on the
grating sensors and so on [1-2]. Among them,
fiber, creating microbendings in the fiber. The
intensity-based sensors enjoy the most simply
change of transfer coefficient ΔT according to the
structure and thus are widely studied in past and
applied pressure force can be described by the
present. However, its application is with limitation
following relationship:
interferometry,
due to its low sensitivity and poor performance towards the source light power fluctuations. In this paper, it is concentrated on investigating the use of optical fiber as a
where kf is the force constant of the bent fiber,
microbending pressure sensor. There are two
which can also be thought of as the effective spring
traditional approaches to optical fiber pressure
constant of the optical fiber, ASYS/lS is a force
sensors are stress induced attenuation [4] and
constant with included distance change of plates.
microbend attenuation [6;7].
As the cross-sectional area of the fiber, Ys is Youngs modulus, ls is the distance length of deformation plates, and ∆T/∆X relates the change in transmission to the change in fiber amplitude due
Microbending Sensor Microbending optical fiber sensors based
to deformation, which depends on the modal
on bend-induced loss in optical fiber have proved
structure of the fiber. The force constant is 2
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Pages 1-8
traditionally defined as ΔT/ΔX which a coefficient
to the accuracy of sensing, maximum load pressure
is expressing the rate of change in transmission
was chosen to prevent damage of the fiber.
distortions to change of amplitude deformation
Laser (He-Ne) wavelength 650 nm is
ΔX. The change in transmission rate will be
launched at one end of the optical fiber. The output
reflected as a change in optical power detected by
power was measured with a power meter (Lambda
the photo detector. This change of output is
LLM-2 Light power source) or recorded as
therefore used to detect changes in physical
intensity spectrum by using spectrometer (Ocean
quantity ΔE. The attenuation in the place of
Optics HR 2000) and the results are displayed on
measurement depends on the pressure force acting
personal computer. The pressure is achieved with
on the sensor. The length of the modulator; the
the help of a mechanical instrument. The pressure
distance length of deformation plates and the
force on the sample increased in steps from (5-50)
mechanical frequency (number of teeth) affect the
N and corresponding outputs are recorded. The
output power measurements.
experiment has been performed under laboratory conditions. Hence, the modulation in output power
Experimental work
is only due to change in pressure on the sample.
A series of permanent microbends is introduced onto a 1m step-index plastic fiber of
Result and discussion
core diameter 380m and numerical aperture 0.3;
In an optical fiber the effect of pressure is
by sandwiching the fiber with a pair of corrugated
mainly confined to the plastic jacket and the cladding.
plates at 10 cm deform cell length and applying
There is little deformation of the core. Hence, if pressure force is increased, the nature of the
moderately high pressures of a few kilograms per
fundamental and other lower order modes changes very
square centimeter. The distance length of
slightly.
deformation plates used to bend the fiber are 6mm
Power transmitted in the optical fiber is
and 8 mm each having a pitch of the corrugation
shared by the core and cladding. With pressure
as 8 mm. A schematic diagram and a photographic
increasing, the coupling takes place between the
picture of the experimental setup is shown in Fig
cladding modes and higher order core modes.
(2).
However, the lower order modes are tightly Deformation plates, made of grooves, allow
concentrated in the core region with little
using the sensor in two models at different lS (6
penetration into the cladding region. This
mm and 8 mm). Input and output part of the optical
wavelength is transmitted through MMF, where
fiber is fixed in foam pieces to prevent damage.
this fiber is passed through microbend cell at 6mm
Mutual positions of plates are fixed. Minimum
or 8mm.
used load pressure force was chosen with respect 3
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Pages 1-8
Fig (3) shows the increase of applied force
increased for two microbend cell models. The
at range from 5N to 50N and the decreased output
intensity at the range of applied force is shown in
power. The reference power means no applied
figure (6). Output intensity is decreased with
force on two microbend cells is 18µw. The output
increased force for both models.
power from (6mm) microband cell change from
Absorbance is dimensionless measurement
18µw to 16.8µw at the force range from 5N to 50
of ability of media to absorb light. Absorbance (A)
N and the output power from the second
occurs when a photon emitted from a light source
microbend cell (8mm) are varies from 60µw to
excites an electron from a ground state to higher
20ن1µw at the same range of applied pressure
energy orbital, it is represented by the following
force .From this figure the output power at 8mm
equation [11]:
microbend cell is less than 6mm microbend cell
Aλ = - log(Iλ/Iλo )
because the 8mm model is greater bend than the
where
6mm model ,that means increased the bend losses.
Aλ is the absorbance at specific wavelength (λ)
Curves ‘blue’ and ‘red’ show that as pressure force
Iλ is the intensity of light at wavelength λ
increases, normalized output power decreases.
Iλo is the intensity of incident light at wavelength λ
The power loss (in percent) of the laser transmitted
before the incidence on the sample.
through the fiber optic as a result of bending deflection was determined from the following
The calculated absorbance of two models
equation [7]:
is shown in fig (7). The absorbance of 6mm is less than 8mm because the second model is being bent greater than the first model and the losses in 8mm
where Pl is the power loss, Ps is the power
is higher.
measured for straight fiber optic, and Pd is the
From all these results the fiber is bent to
power measured for deflected optical fiber of the
critical angle and some modes escaped from the
same length.
core to the cladding. It leads to changes in the
The output power loss of two microbend
intensity of back-scattered radiation in the place of
cells is shown in fig (4).
effect. The plates in response for the change of
From this fig (4) the power loss of 8mm
physical quantity ΔE act by force ΔF on the fiber,
microbend cell is greater than the power loss of
creating microbendings in the fiber. The change of
6mm microbend cell.
transfer coefficient ∆T according to the applied
Intensity spectrum of the laser for different
force can be described by the relationship in
applied force is shown in figure (5). The intensity
equation (1)
spectrum is decreased when the applied force is 4
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Vol. 4 Issue 2 2019 4th Year
The change in transmission rate will
Pages 1-8
100 mm and width 30mm is from 5 to 50N. The
appear as a change in output optical power
sensor was examined in laboratory conditions.
detected by the power meter detector. The loss increases strongly depend on the Conclusions
pressure force, using different pressure force, the
Microbend sensors have many advantages and
less losses possible when the pressure force is (5)
applications in different fields. microbending
N.
effect is considered in multimode fibers as a transduction
mechanism
for
The power and intensity results of 8mm cell at
sensing
different applied force are less than 6mm.
environmental change. An optimized generic microbend sensor was built and utilized to detect applied pressure force. By studying generic design, the microbend sensor is examined for pressure measurements. dynamic range of the sensor for the length of plates
Fig (1) Geometry of microbending cell [4].
5
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Vol. 4 Issue 2 2019 4th Year
Fig (2) (a) schematic diagram and (b)photographic picture of experimental setup.
Fig (3) the output power for two microbend cells.
Fig (4) the power loss for two microbend cells.
6
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Vol. 4 Issue 2 2019 4th Year
Fig (5) the intensity spectrum of two microbend cell 6mm &8mm.
Fig (7) calculate absorbance for two models of laser.
Fig (6) output intensity as a function of applied force.
Reference [3]
[1] J. W. Berthold, “Historical review of microbend
fiber-optic
sensors,”
J. N. Fields and J. H. Cole, “Fiber microbend acoustic sensor,” Appl. Opt.,
J.
vol. 19, pp. 3265–3267, (1980).
Lighwave Technol., vol. 13, pp. 1193–
[4] M. B. J. Diemeer and E. S. Trommel,
1199, (1995).
“Microbend sensors: Sensitivity as a function
[2] J. N. Fields J. H. Cole, “Pressure sensor,”
of distortion wavelength,” Opt. Lett., vol. 9, pp.
J. Acoust. Soc. Amer., vol. 67, pp. 816–
260–262, (1984).
818, (1980).
[5] I. V Denisov, V. A Sedov, N. A. Rybal’chenko,
7
“A
Fiber-Optic
K.U.C.J
Rabi, Dr. Talib and Esam – Design and Construction ……
Microbending Instruments
Temperature and
Vol. 4 Issue 2 2019 4th Year
Sensor”,
Experimental
Techniques, 48(5):683–685, (2005). [6]
H.S.
Efendioglu,
Fidanboylu,
T.Yildirim,
“Prediction
of
K. Force
Measurements of a Microbend Sensor Based on an Artificial Neural Network”, Sensors, 9(9):7167-7176, (2009). [7]
N. Lagakos, R. Mohr, and O. H. ElBayoumi, "Stress optic coefficient and stress profile in optical fibers," Appl. Opt. 20, 2309-2313, (1981).
[8] N. Lagakos, J. H. Cole, and J. A. Bucaro, "Microbend fiber-optic sensor," Appl. Opt. 26, 2171-2180 (1987). [9]
N. K. Pandey, and B.C. Yadav, “Embedded
Fiber
Optic
Microbend
Sensor for Measurement of High Pressure and Crack Detection”, Sensors and Actuators, A 128:33-36,( 2006). [10] G. Murtaza, S. L. Jones, J. M. Senior, and N. Haigh, “Loss Behavior of Single-mode Optical Fiber Microbend Sensors”, Fiber and Integrated Optics, 58:53-58, (2001). [11] Lagakos, N, Cole, J. H., Bucaro, J. A.,"Microbend Sensor", Applied Optics, Vol. 26, pp. 2171-2180, (1987).
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Pages 9-17
مجلة كلية الكوت الجامعة
Vol. 4
Issue 2
2019
4th Year
Study the Optical and Structural Properties SnO2 Films Grown by (APCVD) Nagham T. Ali * and Talib Zeedan T. Al-Mosawi** ** Center of Laser and Optoelectronic –Directorate of Materials Research, Ministry of Science and Technology-Baghdad-Iraq *Physics Department, College of Science, AL-Mustansiriyah University Kut University College Nagam2105@gmail.com Abstract In this research thin films of SnO2 semiconductor have been prepared by using (APCVD) on glass substrates. Our study focusses on prepare SnO2 films with high optical quality at various temperature. The optical transmittance was measured by UV-VIS spectrophotometer. Structure properties were studied by using X-ray diffraction. (XRD) studies; shows the peaks becomes sharper indication to improve the crystallinity, the (110) peak has strongest intensity in all films with increasing growth temperature from (350-500) 0C and the grain size was (31.5nm) which measured by using Scherer equation. (AFM) where use to analyze the morphology of the tine oxides surface, the roughness and average grain size for different temperature have been investigated. Maximum transmission can be measured is (90%) at 400 0C.
الخالصة في هذا البحث تم تحضير أغشية شبه الموصل اوكسيد القصدير بطريقة الترسيب الكيماوي بالبخار بالضغط الجوي االعتيادي . في بحثنا هذا تم التركيز على تحضير أغشية اوكسيد القصدير ذات نوعية بصرية عالية لمختلف درجات الحرارة.على أساس من الزجاج ( أما الخصائص التركيبية فقد تم دراستها باستخدام حيود األشعة السينيةUV-Vis.) تم دراسة الخصائص البصرية للغشاء باستخدام جهاز 9
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( تمتلك أعلى شدة في جميع األغشية بتغيير110) التي أوضحت ان قمم الحيود أصبحت حادة وهذا مؤشر على دعم التركيب ألبلوري القمة لقد تم.( التي تم احتسابها باستخدام معادلة شرر31.5 nm) ( أما الحجم الحبيبي فقيمته كانت350-500) 0C حرارة نمو الغشاء لمدى استخدم مجهر القوى االلكترونية لتحليل طوبوغرافيا سطح أغشية. (4000C) ( عند درجة90%) الحصول على أعظم نفاذية والتي كانت .اوكسيد القصدير وحساب معدل الحجم الحبيبي والخشونة لمختلف درجات الحرارة
However, due to the high intrinsic defects, that is Introduction
oxygen
deficiencies,
tin
oxide
(SnO2−X)
The tin oxide is a wide band gap
possesses a high conductivity. It has been shown
semiconductor (energy bandgap 3.6 eV), and it
that the formation energy of oxygen vacancies and
has only the tin atom that occupies the center of a
tin interstitials in SnO2 is very low. Therefore,
surrounding core composed of six oxygen atoms
these defects form readily, which explains the
placed approximately at the corners of a
high conductivity of pure, but nonstoichiometric,
quasiregular octahedron (Figure 1). In the case of
tin oxide.
oxygen atoms, three tin atoms surround each of
SnO2 thin films have been deposited using
them, forming an almost equilateral triangle. The
different techniques, such as spray pyrolysis [3],
lattice parameters are a = b = 4.737 Å and c =
sol-gel process [4], chemical vapor deposition [5],
3.186 Å [1].
sputtering [6], and pulsed laser deposition [7].
SnO2 is a special oxide material because it has a low electrical resistance with high optical transparency in the visible range. Due to these
Experimental Details
properties, apart from gas sensors, SnO2 is being
The
schematic Pressure
diagram Chemical
of
the
used in many other applications, such as electrode
Atmospheric
Vapor
materials in solar cells, light-emitting diodes, flat-
Deposition APCVD system is given in Fig. (2).
panel displays, and other optoelectronic devices
It contains a tubular furnace which has a diameter
where an electric contact needs to be made
of 50 mm. APCVD is basically a chemical
without obstructing photons from either entering
process which consists of heating hydrated tin
or escaping the optical active area and in
dichloride (SnCl2, 2H2O) under a dry oxygen
transparent electronics, such as transparent field
flow. The vapor of the precursor reacts with
effect transistors [2]. SnO2 owing to a wide band
oxygen then carried on the glass substrate by the
gap is an insulator in its stoichiometric form.
O2 gas.N2 gas use to prevent the oxidation of substrate during heating. The fundamental chemical reaction SnO2 thin films is:
SnCl2 + O2 10
SnO2+ Cl2
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operating parameters shown in table (1)
where D is the crystallite size, λ is the X-ray
(1) N2 gas (2) flow meter (3) furnace (4)spiral
wavelength, β is the full width at half maximum
hater (5) (13)
heater electronic control with
of the diffraction peak, and θ is the Bragg
thermal sensor (K-type) (6) O2 gas (7) flow meter
diffraction angle of the diffraction peaks. The
(8) circular heater (12) sensor with controller (9)
average particle size was found to be (31.5 nm).
byproduct treatment unit (10) (11) substrate and
X-ray diffraction patterns show only five sharp
susceptor.
peaks (110), (101), (200), (211), (220), this evidence polycrystalline of SnO2 in nature.
Table (1) Deposition parameters of tin oxide film
2-Optical properties
Deposition parameters of tin oxide film
SnO2 thin film successfully deposited on
Thin film
SnO2
to glass substrate and thin film were very
Substrate
Glass
transparent. The optical transmission of the
susceptor
Stainless steel
samples is investigated in the range of 280 to
Temperature (0C)
350-500
1100nm using UV-VIS spectrophotometer as
O2 gas flow rate
2L/min
shown in Fig. (4). The measurements are taken in
N2 gas flow rate
0.5l/min
the wavelength scanning mode for normal incidence Transmission spectra show 79-90%
Results and Discussion
transmission in visible and near infrared region.
1-Structural properties by XRD
maximum transmission can be measured is (90%)
XRD
measurement
were
made
at 400 0C.
to
determine the phase, crystallographic structure 3- Surface topography properties
and the grain size of crystallites. X-ray diffraction pattern SnO2 films deposited on glass substrate at
The study of surface morphology of SnO2
various temperature (350-500)oC are shown in
thin films deposited by chemical vapor deposition
Figure (3).The max. peak at 2θ values of 31.85°.
method has been carried out using atomic force
A matching of the observed and standard (hkl)
microscopy (AFM). We report the AFM images
planes confirmed that the product is of SnO2
of SnO2 thin film in three dimensions view 3D. It
having a tetragonal Structure. The average particle
is clear that the deposited layer is very flat. In
size (D) was estimated using the Scherrer
order to have quantitative information about the
equation:
sample topography we analyzed the surface D = 0.9λ / β cos (θ)
heights histogram. figure (5) show typical
11
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roughness and distribution histograms a for(a) 450 0
Pages 9-17
Conclusions
C(b) 500 0C. In figure (6) compares typical
Tin oxide thin film has been successfully
morphology of the SnO2 sample (450-500)0C in
deposited at glass substrate by using CVD
three dimension It can be seen from fig. (5) & (6)
method. Structural investigations using. XRD
that with increasing substrate temperature the
reveal that the layers are composed of SnO2, grain
degree of surface roughness increases.
size was 31.5 nm measured by Scherrer equation. Max. transmittance was 90% in a visible light spectrum, the average roughness of thin film surface is about (1.82- 2.92 nm).
Figure (1) The rutile structure of SnO2 unit cell
Figure (2) APCVD tube furnace system
12
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Figure (3) X-ray diffraction pattern for SnO2 film deposited on glass substrate at various temperature (350-500)0C
120
500 450 400 350
100
T %
80 60 40
20 0 0
200
400 Wave length λ nm
600
Figure (4) transmittance spectra for SnO2 films.
13
800
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Figure (5) : (a) Distribution Report for (450 0C) Sample:450
Code:Sample Code
Roughness Average: 1.82(nm)
Grain No.:47
Instrument:CSPM
Date:2013-03-16
Avg. Diameter:119.74 nm Diameter
Volume
Cumulation
Diameter
Volume
Cumulation
Diameter
Volume
Cumulation
(nm)<
(%)
(%)
(nm)<
(%)
(%)
(nm)<
(%)
(%)
70.00
2.13
2.13
120.00
10.64
48.94
170.00
4.26
93.62
80.00
2.13
4.26
130.00
21.28
70.21
180.00
4.26
97.87
90.00
8.51
12.77
140.00
10.64
80.85
190.00
2.13
100.00
100.00
12.77
25.53
150.00
2.13
82.98
110.00
12.77
38.30
160.00
6.38
89.36
14
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Figure (5) : (b) Distribution Report for (500 0C) Sample: 500
Code: Sample Code Grain No.: 109
Roughness Average: 2.92(nm) Instrument: CSPM
Date: 2013-03-16
Avg. Diameter: 86.31 nm Diameter
Volume
Cumulation
Diameter
Volume
Cumulation
Diameter
Volume
Cumulation
(nm)<
(%)
(%)
(nm)<
(%)
(%)
(nm)<
(%)
(%)
20.00
1.83
1.83
70.00
4.59
31.19
115.00
2.75
77.98
30.00
0.92
2.75
75.00
6.42
37.61
120.00
0.92
78.90
35.00
0.92
3.67
80.00
5.50
43.12
125.00
7.34
86.24
40.00
3.67
7.34
85.00
8.26
51.38
130.00
2.75
88.99
45.00
4.59
11.93
90.00
5.50
56.88
135.00
7.34
96.33
50.00
2.75
14.68
95.00
3.67
60.55
140.00
2.75
99.08
55.00
0.92
15.60
100.00
5.50
66.06
145.00
0.92
100.00
60.00
3.67
19.27
105.00
5.50
71.56
65.00
7.34
26.61
110.00
3.67
75.23
15
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(a) 450 0C
(B) 500 0C
Fig. (6 ) compares typical morphology of the SnO2 sample (450-500)0C in three dimension.
16
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Vol. 4 Issue 2 2019 4th Year
References
Pages 9-17
[5] R. Larciprete, E. Borsella, P. De Padova, P.
[1] R. B. Vasiliev, M. N. Rumyantseva, S. E.
Perfetti, G. Faglia, and G. Sberveglieri,
Podguzova, A. S. Ryzhikov, L. I. Ryabova,
“Organotin films deposited by laserinduced
and A. M. Gaskov, “Effect of interdiffusion
CVD as active layers in chemical gas
on electrical and gas sensor properties of
sensors,” Thin Solid Films, vol. 323, no. 1-
CuO/SnO2
2, pp. 291–295, 1998.
heterostructure,
”Materials
Science and Engineering B, vol. 57, no. 3,
[6] G. Sberveglieri, G. Faglia, S. Groppelli, and P. Nelli, “Methods for the preparation of
pp. 241–246, 1999. [2] J. F. Wager, “Transparent electronics,”
NO, NO2 and H2 sensors based on tin
Science, vol. 300, no. 5623, pp. 1245–1246,
oxide thin films, grown by means of the r.f.
2003.
magnetron sputtering technique,” Sensors
[3] S. D. Shinde, G. E. Patil, D. D. Kajale, V. B.
and Actuators B, vol. 8, no. 1, pp. 79–88,
Gaikwad, and G. H. Jain, “Synthesis of ZnO
1992.
nanorods by spray pyrolysis for H2S gas
[7]
sensor,” Journal of Alloys and Compounds,
R. Dolbec, M. A. El Khakani, A. M. Serventi, and R. G. SaintJacques, “Influence of the nanostructural
vol. 528, pp. 109–114, 2012. [4] C. Cobianu, C. Savaniu, P. Siciliano, S.
characteristics
on
the
gas
sensing
Capone, M. Utriainen, and L. Niinisto,
properties of pulsed laser deposited tin
“SnO2 sol-gel derived thin films for
oxide thin films,” Sensors and Actuators
integrated gas sensors,” Sensors and
B, vol. 93, no. 1–3, pp. 566– 571, 2003.
Actuators B, vol. 77, no. 1-2, pp. 496–502, 2001.
17
Meriam – Comparison of Antibacterial …….
ISSN (E) : 2616 – 7808
I
ISSN (P) : 2414 - 7419
K.U.C.J
Vol. 4 Issue 2 2019 4th Year
Pages 18-28
مجلة كلية الكوت الجامعة
Vol. 4
Issue 2
2019
4th Year
Comparison of Antibacterial Effect of Biosynthesis Nanoparticles with Chemically Synthesis Nanoparticles in Vitro Meraim A. Kazaal Al Kut University College, Department of techniques of pathological analysis, Al-Kut. Iraq meraim1162018@gmail.com
ABSTRACT The continuation emergence of multidrug resistant bacterial infections and the decline in discovery of new antibiotics are main challenges for health care throughout the world. Recently, chemically and biologically synthesis nanoparticles are used as new antimicrobial agents. Present study focused on detection antimicrobial action of biosynthesis nanoparticles versus chemically synthesis nanoparticles on bacterial infections in Lab. Method: in this study, zinc oxide nanoparticles (ZnONPs) and silver nanoparticles (AgNPs) are produced from zinc nitrate and silver nitrate respectively by chemical and biological methods. One concentrations of metallic nanoparticles (60ppm) are tested against salmonella typhi (S. typhi), Pseudomonas aeruginosa (P. aeruginosa), Streptococcus pneumonia (S. pneumonia) and Streptococcus aureus (S. aureus) by disc diffusion method. Result: biologically synthesis AgNPs more effected on bacterial species (especially on S. pneumonia) than biologically synthesis ZnONPs, chemically synthesis ZnONPs and chemically synthesis AgNPs. On other hand biologically synthesis ZnONPs more effected than chemically synthesis ZnONPs on bacterial species especially S. pneumonia. Conclusion: biologically synthesis nanoparticles more effected on tested bacterial species especially S. pneumonia then chemically synthesis nanoparticles. Biologically synthesis AgNPs are an excellent antimicrobial agent. Keyword;
AgNPs,
ZnONPs,
salmonella
typhi,
pneumoniae, Streptococcus aureus. 18
Pseudomonas
aeruginosa,
Streptococcus
Pages 18-28
K.U.C.J
Vol. 4 Issue 2 2019 4th Year
Meriam – Comparison of Antibacterial …….
مقارنة التأثير المضاد للبكتيريا لجسيمات النانوية المصنعة حياتيا مع الجسيمات النانوية المصنعة كيميائيا في المختبر د .مريم عطية خزعل قسم التحليالت المرضية /كلية الكوت الجامعة /واسط /العراق الخالصة استمرار ظهور االصابات البكتيرية المتعددة المقاومة ألدوية والتراجع في اكتشااام مدااادات يياجيااة جدياادة م ا التحااديات ال ااحية الرئيسية التي جواجة العالم .مؤخرا الجسيمات النانويااة الم اانعة كيميائيااا او ييويااا اسااتتدمد كداادات جدياادة للجااراميم .الدراسااة الحالية ركزت على جحديد التأمير المثبط لجزيئات النانوية الم نعة يياجيا عكس الجزيئات النانوية الم اانعة كيميائيااا .طريققا العمققل: في هذة الدراسة الجسيمات النانوية ألوكسيد لزنااو و الةدااة انتجااد ما نتاارات الزنااو و نتاارات الةدااة ب ريقااة كيميائيااة وطريقااة يياجية .جركيز وايد( (ppm60م الجساايمات النانويااة المعدنيااة اختباار ضااد salmonella typhi (S. typhi), Pseudomonas aeruginosa (P. aeruginosa), Streptococcus pneumonia (S. pneumonia) and Streptococcus aureus (S. ) aureusب ريقااة االنتشااار القرصااي .النتققائ
الجساايمات النانويااة للةدااة اكتاار جااأميرا علااى االنااوا( البكتيريااة ( باااألخ
( S.
)pneumoniaم الجسيمات الناوية للةدة الم نعة كيميائيا و الجسيمات النانوية ألوكسيد الزنو الم اانعة كيميائيااا او يياجيااا .م ا ( )S. pneumoniaم ا
جهة اخرى الجسيمات النانوية ألوكسيد الزنو الم نعة يياجيا اكثر جأمير على االنوا( البكتيرية ( باألخ
الجسيمات النانوية ألوكسيد الزنو الم نعة كيميائيا .الخاتمة :الجسيمات النانوية الم نعة بال ريقة الحياجية اكثر جثبي ا لنمو االنااوا( البكتيرية ( باااألخ
)S. pneumoniaما الجساايمات النانويااة الم اانعة بال ريقااة الكيميائيااة .الجساايمات النانويااة للةدااة يمك ا
اعتبارها مداد ممتاز للجراميم .
INTRODUCTION extracts is an interesting area in the field of
Drug resistance by pathogenic bacteria
nanotechnology, which has economic and eco-
remain worldwide problem [1]. Therefore, we
friendly benefits over chemical and physical
require to find out novel strategies or recognize
methods of synthesis [3].
new antimicrobial agents to control microbial
Nanoparticles (NPs) are typically no
infections. Superior effectiveness on resistant
greater than 100 nm in size and their biocidal
strains of microbial pathogens, less toxicity and
effectiveness is suggested to be owing to a
heat resistance are the characteristic of metal
combination of their small size and high
nanoparticles, which make them the selective
surface-to-volume ratio, which enable intimate
[2].
candidates
interactions with microbial membranes. In
Biosynthesis of green nanoparticles using plant 19
bacteria
eradicating
for
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addition, inorganic antibacterial agents such as
antimicrobial efficacy is greatly enhanced.
metal
advantageous
Though Ag-NPs find use in many antibacterial
compared to organic compound due to their
applications, the action of this metal on
stability
microbes is not fully known. It has been
and metal
[4].
oxides are
Among
these
metal
oxides, ZnO has attracted a special attention as
hypothesized
antibacterial agent. For instance, ZnO inhibits
cause cell lysis or growth inhibition via various
the adhesion and internal-ization gram negative
mechanisms [9,10]. The lethality of silver for
bacteria. In addition, ZnO nanoparticles exhibit
bacteria can also be in part explained by thiol-
antibacterial activity and can reduce the
group reactions that inactivate enzymes [11].
attachment and viability of microbes on
that silver
Several
reports
nanoparticles can
demonstrated
the
biomedical surfaces [5]. Interestingly, several
synthesis of ZnO- and Ag-NPs from natural
results suggest a selective toxicity of ZnO-NPs
sources like plants or microorganisms by green
preferentially
targeting prokaryotic systems,
chemistry approaches [12]. The use of plant
although killing of cancer cells has also been
extracts for nanoparticles synthe-sis may be
demonstrated [6]. Several mechanisms have
advantageous over other biological processes,
been reported for the antibacterial activity of
because it drops the elaborate process of
ZnO-NPs. For example ZnO-NPs can interact
maintain-ing cell cultures and can also be used
with membrane
for
lipids and
disorganize
the
large-scale
NPs
synthesis
[13].
membrane structure, which leads to loss of
Additionally, the green chemistry approach for
membrane integrity, malfunction, and finally to
the synthesis of NPs using plants avoids the
bacterial death [7]. ZnO may also penetrate into
generation of toxic byproducts. Among the
bacterial cells at a nanoscale level and result in
various
the production of toxic oxygen radicals, which
mediated NPs synthesis is preferred as it is
damage DNA, cell membranes or cell proteins,
cost-effective,
and may finally lead to the inhibition of
human therapeutic use [14]. In present study,
bacterial growth and eventually to bacterial
we compared between antibacterial action of
death [8].
biosynthesis
Silver is generally used as nitrate salt,
known
synthesis
eco-friendly
nanoparticles
methods,
and
and
safe
plant
for
chemically
synthesis nanoparticles on some bacterial
but in the form of Ag nanoparticles (Ag-NPs)
infections.
the surface area is increased and thereby
20
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MATERIALS AND METHODS
Pages 18-28
hydride (NaBH4). To stabilize the solution, 0.3% polyvinyl pyrolidine (PVP) was added to
Sample
preparation:
collected from
Different
samples
the solution to prevent the particles density.
patients in Al-Diwaniya
The size of nanoparticles in the zinc or silver
teaching hospital. Bacterial species (S. typhi, P.
nanoparticle suspension were determined by
aeruginosa, S. pneumonia and S. aureus) are
SALD2101. Suspension of zinc or silver
isolated and identified by culture media and
nanoparticles became lyophilized powder by
biochemical test in bacteriology laboratory in
freeze-drying method and were kept in a closed
Al-Diwaniya teaching hospital.
container in the refrigerator at 4°C [15].
Biological synthesis of nanoparticles: Nerium Bacterial susceptibility to nano-particles:
oleander leaves have been washed and left to
One concentrations (60 ppm) from each of
dry at room temperature for 4 days and then
chemically synthesis and biosynthesized nano-
sliced into pieces. 10 gram of the leaves have
particles are tested against S. typhi, P.
been weighed and placed in a flask with 100 ml
aeruginosa, S. pneumonia and S. aureus in this
distilled water and then boiled for about 5
study. To examine the susceptibility of
minutes, filtrated by filter paper and left to
bacterial species to different nano-particles
chill. 7 ml of the extract were added to an
concentrations, Muller Hinton agar are used.
Erlenmeyer flask containing 100 ml of 1mM
Muller Hinton agar were prepared with holes,
Silver nitrate or zinc nitrate. The reaction was
the diameter for each hole was 5 mm. In each
performed at room temperature and darkness.
hole, 0.2 ml of chemically synthesis and
The reduction of silver and zinc ions was
biosynthesized nanoparticles are placed (with
indicated by the transformation of the color
three replications for each test). Put the plates
into brown which gives us primal evidence of
in the incubator for 24 hrs. in temperature of
the formation of nanoparticles. A sample of the
37°C then zone of inhibition was measured
mixture has been analysed by :Uv -vis spectra,
manually. In additional, dimethyl sulfoxide
X-ray Diffraction (XRD) , Energy dispersive
(DMSO) is placed in other holes as control.
spectro-scopy (EDS) and Scanning electron microscope (SEM) to characterize the formed nanoparticles.
RESULTS Chemically
synthesis
of
The
nano-particles:
effect
of
chemically nanoparticles
synthesis on
and
Chemical reduction method was used for
biosynthesized
bacterial
synthesis of nanoparticles by Sodium Boron
species growth can be seen in figure (1). Table (1) showed that AgNPs significantly inhibited
21
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growth of bacterial species (p <0.05) in
active against tested bacterial species then
compared
Moreover,
chemically synthesis nanoparticles this may be
biosynthesized AgNPs are more effected on
due to different in properties of produced
bacterial species than chemically synthesis
nanoparticles. The high surface to volume ratio
AgNPs especial on gram positive bacteria
of nano-particles plays an important role in
(mean of zone of inhibition 31mm and 29mm
inhibiting the growth of bacteria. Bactericidal
for S. pneumonia and S. aureus respectively) as
effects of nanoparticles is influenced by the
in figure (2). Also, ZnONPs have high
particle diameter. Therefore, the choice of
antimicrobial effect on bacterial species in
synthesis method is effective for controlling the
compared with chemically synthesis ZnONPs
size of nanoparticles [18,19]. The small
especial on gram positive bacteria (mean of
particles were more antibacterial and had more
zone of inhibition 28mm and 26mm for S.
antibiofilm activity than large particles, as well
pneumonia
respectively
as, the antimicrobial activity of triangular-
(figure3). Biosynthesized AgNPs the best
shaped nanoparticles more than spherical
inhibitor for bacterial growth (especially S.
particles. In the past, studies also reported that
pneumonia) in compared with chemically
antimicrobial activity depends on the size of
synthesis
synthesis
the nanoparticles [20]. Similar to our data,
ZnONPs and biosynthesized ZnONPs. In
Doudi et al. (2011) and Ruparelia et al. (2008)
contrast to S. pneumonia, P. aeruginosa are
reported that gram negative bacterial species
less effected by nanoparticles (zones of
had a higher resistance to silver nanoparticles
inhibition are 21mm, 20mm, 26mm and 13mm
than gram positive bacterial species. Some
for Biosynthesis AgNPs, Chemo- AgNPs, Bio-
researcher believe that lipopoly-saccharide of
ZnONPs and Chemo -ZnONPs respectively)
Gram-negative bacteria trap positively charged
with
and
control.
S.
AgNPs,
aureus
chemically
silver nano-particles and lead to the blocking of nanoparticles [21,22]. As a result, antibacterial activity of silver nano-particles needs to reach
DISCUSSION
the
cell
membrane.
In
fact,
the
silver
Several approaches have been employed to
nanoparticles are attached to the surface of cell
improve the methods for synthesizing Ag- and
membranes and can disrupted the performance
ZnO-NPs including chemical and biological
of the membrane, penetrate the cell and release
methods. Recently, nanoparticles synthesis
silver ions [21,22,23]. Ghotaslou et al.,(2017)
based on plant extracts is becoming more
showed the effect of silver nanoparticles
popular [16,17]. In line with other studies
against
[17,18,24],
present
Staphylococcus
biologically
synthesis
study
showed
nanoparticles
that more
Escherichia
coli
aureus
was
and
less
than
Pseudomonas
aeruginosa [18]. Salema and his coworkers
22
K.U.C.J
Meriam – Comparison of Antibacterial …….
Vol. 4 Issue 2 2019 4th Year
Pages 18-28
(2015) demon-strated that a single oral
However, molecular studies are needed to
administration of silver nanoparticles to infant
reveal the clear evidence of toxic mechanisms
mice colonized with V. cholerae or ETEC
that will be correlated to ZnONPs and AgNPs.
significantly reduces the colonization rates of
Also
the pathogens by 75- or 100-fold, respectively
mutagenicity and carcinogenicity are required
[4]. Furthermore this data agreement with study
to clarify any adverse effects of nanoparticles
of Salema his coworkers (2015) who found
and support the safe use for them.
studies
about
long-term
toxicity,
that AgNPs more effected on bacteria then ZnONPs [4] this may be related to natural, size,
CONCLUSION
shape and other antimicrobial properties of
cally synthesis nanoparticles more effected on
AgNPs
compared with ZnONPs [25,26,27].
tested bacterial species especially S. pneumonia
Oberdorster et al., (2005) demon-strated that
then chemical synthesis nanoparticles. In
the size, shape, surface area, solubility,
contrast to S. pneumonia, P. aeruginosa are
chemical composition and dispersion factor of
less effected by nanoparticles Biologically
nanoparticles
play
exceptional
roles
synthesis AgNPs are an excellent antimicrobial
determining
their
biological
responses
in
agent.
[28,29,30].
A
B 1
4
C
4
2
3
Control 2
3
D 4
4
3
control 1
3
2
1
1
2
Figure (1): effect of nanoparticles on bacterial species: A= S. aureus, B= P. aeruginosa, C= S. pneumonia and D= S. typhi (1= Biosynthesis AgNPs, 2= ChemoAgNPs, 3= Bio-ZnONPs and 4= Chemo -ZnONPs
23
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Table (1): show bacterial sensitivity to zinc and silver nanoparticles Zone of inhibition (mm) (mean ±SD) Bacterial
Biosynthesi
Chemo-
Bio-
Chemo
Control
Species
s -AgNPs
AgNPs
ZnONPs
ZnONPs
(DMSO)
(60 ppm)
(60 ppm)
(60 ppm)
(60ppm)
S. typhi
25±3.88**
19±5.11**
20±1.87**
15±3.09*
0±0
P. aeruginosa
21±5.10**
20±3.211**
26±4.0**
13±6.21*
0±0
S. pneumonia
31±1.99**
22±5.01**
28±1.83**
17±5.74*
0±0
S. aureus
29±5.09**
19±3.64**
26±4.71**
12±1*
0±0
Significant association (p <0.05) in compared with control, **= Significant association (p<0.001) in compared with control, SD = Standard Deviation, NS= Not Significant (p > 0.05).
Figure (2): show compared between antimicrobial effect of chemically synthesis and biosynthesized AgNPs on tested bacterial species
Figure (3): show compared between antimicrobial effect of AgNPs and biosynthesized ZnONP s on tested bacterial species.
24
K.U.C.J
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Vol. 4 Issue 2 2019 4th Year
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Figure (4): show compared between antimicrobial effect of chemically synthesis and biosynthesized nanoparticles on tested bacterial species.
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K.U.C.J
Mohammed, Mohammed and Haneen – Concentration and …….
ISSN (E) : 2616 – 7808
I
ISSN (P) : 2414 - 7419
Vol. 4 Issue 2 2019 4th Year
Pages 29-37
مجلة كلية الكوت الجامعة
Vol. 4
Issue 2
2019
4th Year
Concentrations and [pH] Effects on Spectral Shifts of C6H6 and CCl4 Compounds 1
Mohammed S. Mahde, 2M. R. Mohammad , 3Haneen Muthanna Awad Al- Karkh University for Science College of Science , Baghdad – IRAQ
2,3
Applied Sciences Department - University of Technology , Baghdad – IRAQ 1 2
mosame_11@yahoo.com
d_mohamed11@yahoo.com 3
randa5794@yahoo.com
Abstract: The electronic spectra within UV-Vis region for benzene (C6H6) and Carbone tetrachloride (CCl4) molecules have been studied. Since Benzene molecule belongs to D6h point group, with very high symmetry elements, therefore it may be expected for its internal vibrations to be either infrared or Raman active only. The spectral properties of (CCl4) are also have been studied. This (CCl4) belongs to Td point group, where its fundamental internal vibrations will be also, infrared or Raman actives. These aspects will be considered and discussed in this work. Keywords: CCl4 molecules, FTIR, Raman spectroscopy.
خصائص اإلزاحة الطيفية عند تراكيز وقيم مختلفة لالس الهيدروجيني لمحاليل البنزين ورابع كلوريد الكاربون حنين مثنى عواد2 محمد راضي محمد و2 ، محمد صالح مهدي1 بغداد- العراق، جامعة الكرخ للعلوم1 بغداد- العراق، الجامعة التكنلوجية، قسم العلوم التطبيقية2
الخالصة .تمت دراسة االطياف االلكترونية ضمن منطقة األشعة فوق البنفسجية والمرئية لجزيء البنزين ورابع كلوريد الكاربون لذلك فمن المتوقع ان تكون االهتزازات، ويمتلك عناصر تناظر عالية جدا،D6h نظرا الن جزيء البنزين ينتمي الى المجموعة النقطية .الداخلية األساسية إما نشطة باألشعة تحت الحمراء او الرامان فقط 29
K.U.C.J
Mohammed, Mohammed and Haneen – Concentration and …….
Vol. 4 Issue 2 2019 4th Year
Pages 29-37
حيث تكونTd ) الى مجموعة النقطيةCCl4( ينتمى هذا الجزيء،كما تمت دراسة االطياف االهتزازية لرابع كلوريد الكاربون .اهتزازاتها الداخلية األساسية هي أيضا نشطة في االشعة تحت الحمراء او رامان
1. Introduction The benzene is an aromatic molecule which
The carbon tetrachloride belongs to Td point
consists of six carbon atoms to form the
group, which has the following symmetry
hexagonal ring where each Carbon atoms is
elements, eight axes of rotations by 120 o (3C2),
linked to hydrogen atom. All these twelve atoms
six planes of reflection, three axes of rotation by
are located within a plane, therefor the benzene
180 o, and four of rotation by 180 o + 6 planes of
molecule belongs to the point group D6h ,which
reflections [1].
possesses the followings symmetry elements : -
The internal vibrations are equal (3N-6) where
One axis of rotation at an angle 60o (1C6)
N represents the number of atoms, within the
perpendicular to the plane of the molecule ,Six
molecule.
axis of rotations at 180o (6C2), located at the
Accordingly, the internal vibrations for C6H6
molecular plane and vertical on axis C6, six
molecule would be thirty vibrations (some of
planes of reflection (σv) perpendicular to the
them are single and double degenerates), either
molecule plane ,one plane of reflection (1 σh)
infrared Or Raman actives depending on
applies perpendicular on the plane of the
changing of dipole moment or polarizability
molecule, and one axis of rotation of an angle of
tenser respectively.
180o (1C2) per level the molecule, and one axis
However, for CCl4 molecules, the internal
of rotation by angle of 120o (1C3) is also
vibrations are nine (some of them are single and
perpendicular to the level of the molecule and
triple degenerates).
one analog element for a rotational axis -
These internal vibrations are either infrared or
reflective (S6) and finally one inversion element,
Raman actives depending on changing of dipole
C6H6 is considered to be a non-polar solvent
moment or polarizability tenser respectively.
[1,2].
It should be noted that the external vibrations of
CCl4 is also considered to be a non-polar solvent
the nonlinear molecules (including C6H6 and
as it doesn’t express any permanent molecular
CCl4) are; which are beyond six vibrations, three
dipole moment. This feature is very important in
translational and three rotational vibrations
the spectral studies in the cases of using carbon
[6,7].
tetrachloride as a dilute solvent for some polar
The aims of this work are to study the
substances such as methanol and acetone [3-6].
vibrational
prop
and
electronic
spectral
properties by using infrared and Raman techniques, as well as electronic properties as
30
K.U.C.J
Mohammed, Mohammed and Haneen – Concentration and …….
Vol. 4 Issue 2 2019 4th Year
Pages 29-37
function of concentration and [pH] values of
Mw= 78.11 (gm/mole)
solution of C6H6 and CCl4 molecules.
Different concentrations, which have been used in this work, where calculated by using equation
2.
MATERIALS
AND
EXPERIMENTAL
(2); [M1] V1 = [M2] V2 … (2)
TECHNIQUES 2.1 Chemicals and reagents
where, [M1] is the high concentricity, V1 is the
1. Different chemicals and reagents which have
volume before diluted, [M2] is the low
been used in this study are listed in table
concentration, and V2 is the the volume after
(I). The table is also listed the chemical
diluted. Table (II) is listed nine concentrations
purities, and manufacture compunies and
of C6H6, which have been used in this work.
counteries. Table II: Different concentrations of
Table I: Chemical and regents, which have
Benzene in carbon tetrachloride solvents
been used in this study.
Number
C2(M)
of
V1
V2
(Volume of
(Volume of
C6H6) ml
C6H6+CCl4 ) ml
Chemical
Company
Country
purity
Benzene
BDH
England
98.4%
Carbon
Fluka .Ga
Switzerland
99.5%
tetrachloride
Sample
Ethanol
sigma Aldrich
USA
99.9%
1.
0.1
0.224
25
NaOH
BDH
England
99.9%
2.
0.2
0.449
25
HCl
Romil
UK
99.9%
3.
0.3
0.674
25
4.
0.4
0.899
25
5.
0.5
1.12
25
6.
0.5
1.12
25+drops (HCl)
7.
0.5
1.12
25+drops of
2.3.
Carbon tetrachloride to diluted in
Benzene Equation (1) has been used to dilute the
(NaOH) 8.
0.6
1.3
benzene in carbon tetrachloride solvents, where
25
M1 is equal to ten molarity as listed in table (III). 9.
0.01
0.022
25
M =sp.sr x % x 1000/ Mw … (1) 2.2. Benzene diluted in carbon tetrachloride
CCl4 (purity % ) = 99.5
The concentration of Benzene in carbon tetrachloride solvent in unit of molarity has been
And the Carbon Tetrachloride specific density
measured by using equation (1);
(Sp.sr) = 1.586 gm/cm3
M =sp.sr x purity % x 1000/ Mw … (1)
Mw= 153.81 (gm/mole)
C6H6 (purity %) = 99.8 % [M1] V1 = [M2] V2 … (2)
And the Benzene specific density (Sp.sr) = 0.87 gm/cm
3
31
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Mohammed, Mohammed and Haneen – Concentration and …….
Vol. 4 Issue 2 2019 4th Year
Where, [M1] is the high concentricity, v1 is the
3. Results and discussions
volume before dilution, [M2] is the low
3.1. The results of C6H6 molecule
concentricity, and V2 is the total magnitude after
Pages 29-37
3.1.1. Infrared spectrum
dilution.
The chemical structures and nomenclature for mono- and disubstituted benzene rings, show
Table III: Different concentrations of
how the presence or absence of the ring bend,
carbon tetrachloride in Benzene Solvents. V1
V2
and the position of the out-of-plane aryl C-H wag together can be used to distinguish mono-,
Number
C2(M
(Volume of
(Volume of
of
)
CCl4)
CCl4+C6H6 )
Ml
ml
These peak positions are summarized, both
samples
ortho-, meta-, and para-isomers from each other.
1.
0.1
0.29
25
mono- and meta-isomers have the ring bend
2.
0.2
0.58
25
present and have C-H wagging peaks [8].
3.
0.3
0.88
25
4.
0.4
1.17
25
5.
0.5
1.46
25
6.
0.6
1.75
25
7.
0.01
0.03
25
The FTIR spectrum of benzene has absorption peaks caused by vibrations of aromatic C-C, C=C and C-H bonds. Fig (1) shows the infrared spectrum of benzene, it also shows the assignments of most of the shown bands. The strong absorption band at the
2.4. The UV-Visible spectra have been
range (3600-3300) cm-1 is due to the stretching
measured by using Perkin -Elmer
C-H bond while, the absorption bands belongs
lambda 750, (Germany).
to the stretching and bending vibrations of the
2.5.
Fourier
Transform
functional
Infrared
where a similar bands have been observed by
Spectroscopy (FTIR) Measurements: Fourier
transform
infrared
groups of the benzene molecule,
many researchers [9-13].
spectrometer
(SHIMADZO IRAFFINITY- Japan) has been used. To measure Infrared spectra of, C6H6
100 90 80 70 60 50 40 30 20 10 0
solution and CCl4 compound.
%Transission
2.6 The Raman Spectroscopy:
Benzene
The Raman spectra have been measured by using ventana spectrophotometer, which is used the second harmonic generation laser (532nm) of the Nd-Yag laser as an excitation source. 2.7 [pH] value measurments
C
CC
C-H C-H
stretc h
stretc
400 800 12001600200024002800320036004000
[pH] value measurments have been recorded by
wavenumber(cm-1)
using pH meter type Hana, (Mauritius ) .
Figure 1: FTIR spectra for (C6H6).
32
K.U.C.J
Mohammed, Mohammed and Haneen â&#x20AC;&#x201C; Concentration and â&#x20AC;Śâ&#x20AC;Ś.
The IR spectra of Benzene molecule show
Vol. 4 Issue 2 2019 4th Year
12000
Benzene
-1
pieces between 800-3600 cm , as shown in
Pages 29-37
10000
Intensity (a.u.)
figure (1). These observed bands are due to
8000
active fundamental and combination bands [10].
6000
The infrared spectrum of the molecule shows
4000
only the active infrared fundamental and combination bands. However, no overtone
2000
bands have been detected within this region
0 500
because of the high symmetry of this molecule
1000
1500
2000
2500
3000
3500
Raman shift (cm-1)
[1].
Figure 2: Raman Spectrum of (C6H6).
3.1.2. Raman spectrum of Benzene
3.1.3. UV-Visible spectra of Benzene
The growth in Raman last year continues, with
The UV-Vis spectrum of C6H6 is shown in Fig
ongoing improvements in the tools and a
(3) the band center at 270 nm is assigned to
number of new systems being launched. New
Ď&#x20AC;â&#x2020;&#x2019;Ď&#x20AC;* electronic transition of C=C. 270 nm is
generations of small Raman spectrometers
assigned to Ď&#x20AC;â&#x2020;&#x2019;Ď&#x20AC;* electronic transition of C=C
continue to appear. Both commercial and
[17].
academic users of Raman are seeing more laser, detector, and optical options [14].
Absorbance
Fig (2) shows the Raman spectrum of benzene. This spectrum shows about five bands centered at 606, 996, 1177, 2950 and 3063cm-1 for the vibrations of the above-mentioned bonds. Usually the vibration bands at 2950, and 3063cm
-1
0.7 0.6 0.5 0.4 0.3 0.2 0.1 0 200
due to stretching vibration of C-H,
Benzene
Ď&#x20AC;â&#x2020;&#x2019;Ď&#x20AC;*
300
400
500
đ?&#x153;&#x2020; (nm)
600
700
800
while the bands center at 1177, 996, due to C=C Figure 3: The UV-Visible Spectrum of pure
and C-C stretching vibrations. The band centered at 606 cm-1
C6H6 compound.
is due to out of plain
rocking vibration of C-H [15-16]. the absorption peak wavelength tends to be shifted toward the long wavelength region and the absorption peaks tend to be larger. The absorption peak of Benzene at 275nm. The ultra-violet region shows only bands belong to Ď&#x20AC;â&#x2020;&#x2019;Ď&#x20AC;* electronic transitions single bands C-H and C-C and also Ď&#x20AC;â&#x2020;&#x2019;Ď&#x20AC;* electronic transitions of type electronic double bounded C=C. 33
K.U.C.J
Mohammed, Mohammed and Haneen â&#x20AC;&#x201C; Concentration and â&#x20AC;Śâ&#x20AC;Ś.
Vol. 4 Issue 2 2019 4th Year
Pages 29-37
However, no absorption has been observed
Benzene
300
within visible region (200-800) nm which is
250
confirmed since pure benzene liquid has
200
đ?&#x153;&#x2020;(nm)
colorless [18].
150 100
3.1.4. Changing of the [pH] values of the
50
solvent with Benzene
0 0
In Figure (4) a few changes in the spectra of C6H6 compound have been obsorved when
5
10
[pH]
15
Figure 5: The wavelength Shift of Ď&#x20AC;â&#x2020;&#x2019;Ď&#x20AC;*
NaOH is added. However, no change was
band for C6H6 compound.
abserved when HCl was add. The absorption spectrum exhibits a broad band centered at 270
3.1.5. Changing of concentrations of benzene
nm.
Fig (6) shows the UV-Visible Spectra of (C6H6) at different concentrations. The Ď&#x20AC;â&#x2020;&#x2019;Ď&#x20AC;*
broad
band has been seen at 275 nm at high 0.8
concentration (0.01 M), the broad band has been
0.6 0.5
NaOH , PH =10
shifted to 270 nm, which means blue shift on
0.4
pH=7
diluting of the solution [19]. 4
0.3 0.2
C2=0.1 M C2=0.2 M C2=0.3 M
Benzen
3
Absorbance
Absorbance
concentrations (0.5M), while at the low
HCl, PH=3
0.7
2
0.1
1
0 250
270
290
310
330
đ?&#x153;&#x2020; (nm)
0
350
-1
250
270
đ?&#x153;&#x2020; (nm)
290
Figure 4: The UV-Visible spectra of C6H6 at
Figure 6: The UV-Visible Spectra of
different pH values.
different concentrations of C6H6.
On changing [pH] values of the solution, it
3.2.1.
should be noted that there is no wavelength shift has been observed for the Ď&#x20AC;â&#x2020;&#x2019;Ď&#x20AC;
*
Infrared
Spectra
of
Carbon
tetrachloride.
band of C6H6 The infrared spectrum of CCl4 compound is
Compound, as shown in figure (5).
shown in Fig (7). The point group of CCl4 is Td with high symmetry, therefore one would expect 34
K.U.C.J
Mohammed, Mohammed and Haneen â&#x20AC;&#x201C; Concentration and â&#x20AC;Śâ&#x20AC;Ś.
the vibrations of this molecule to be either IR or
3.2.3.
Raman active. The IR of figure 7 is in good
Vol. 4 Issue 2 2019 4th Year
UV-Visible
spectra
Pages 29-37
of
Carbon
Tetrachloride
agreement with that previously reported [20].
The UV-Vis spectrum of CCl4 is shown in Fig
However, the strong band centered at 1028 cm-1
(9). The only band centered at 280nm is
is the anti-symmetric stretching vibration of
assigned to Ď&#x192;â&#x2020;&#x2019;Ď&#x192;* electronic transition of C-Cl.
CCl4.
This indicates that this compound is colorless
%Transmission
100
since there is no band is obsorved within visible
Carbon tetrachloride
80
region. It should be mentioned that there is no
60 40
wavelength shift is observed, for this band on
20
changing [pH] values.
0
C 400 800 12001600200024002800320036004000
So, the behaver of Ď&#x192;â&#x2020;&#x2019;Ď&#x192; * electronic transition of
Wavenumber (cm-1)
CCl4 is similar to Ď&#x20AC;â&#x2020;&#x2019;Ď&#x20AC;* of C6H6 which has been mentioned earl ear [23].
Figure 7: FTIR spectraum of CCl4.
3.2.2.
Raman
spectra
of
Carbon
0.7
Ď&#x192;â&#x2020;&#x2019;Ď&#x192;
0.6
Tetrachloride
Carbon
0.5
Absorbance
Fig (8) Shows the Raman spectrum of CCl4
0.4
which shows only the symmetric stretching and
0.3
bending only, since these modes of vibrations
0.2
produce change in magnitude of polarizability
0.1
tenser [21-22].
0
Carbon Tetrachloride
Intensity (a.u.)
10000 8000
200
300
400
600
700
800
đ?&#x153;&#x2020; (nm)
Ď&#x2026;1(a1)
6000
Figure 9: The UV-Visible Spectrum of pure
Ď&#x2026;4(t2) Ď&#x2026;3 (t2)and Ď&#x2026;2 Ď&#x2026;1+Ď&#x2026;4(t2)
4000
500
CCl4 compound.
2000 0 0
800
1600
2400
3200
4000
3.2.4.
Raman shift(cm-1)
vibration
ν1(symmetric
of
concentration
of
Carbontetrachloride.
Figure 8: Raman Spectrum of CCl4. The
Changing
Fig (10) shows the UV-Visible Spectra of
stretching
(CCl4) at different concentrations. The Ď&#x192;â&#x2020;&#x2019;Ď&#x192; *
vibration), and the vibration ν2(symmetric
broad band has been seen at 280 nm for
bending) are Raman active only, while ν3 (anti-
all
concentrations, which means that there is no
symmetric stretching vibration), and ν4 (anti-
wavelength shifts were observed on change the
symmetric bending) are Infrared active only.
concentrations [23]. 35
K.U.C.J
Mohammed, Mohammed and Haneen â&#x20AC;&#x201C; Concentration and â&#x20AC;Śâ&#x20AC;Ś.
Vol. 4 Issue 2 2019 4th Year
[4] K. Kayed and 4
Deformity
Carbon Tetrachloride 2 1 0
Absorbsion
3
200
250
300 đ?&#x153;&#x2020; (nm)
Pages 29-37
Mayada Issa, (The
Vibrations
of
Carbon
C2= 0.1
Tetrachloride in Alcoholic Environment),
C2= 0.2
Research) Vol.6, No.5, (2014), 2739-2743.
(International Journal of Chem.Tech.
[5] M.Grazia Giorgini, M. Musso, H. Torii, (J.Phys. Chem A.) 109 (2005) 5846-
350
5854.5. [6] N. E. Levinger, P. Davis, M. Fayer, (Journal
Figure 10: The UV-Visible Spectra at
of Chemical Physics) ,115 (2001) 20-22.
different concentrations of Carbon
[7] P.Musalidhar, and G.Ramana, Indian
Tetrachloride (CCl4).
(Journal of pure and Applied physics), Vol 23, 1,(1985),222-224.
4. Conclusions
[8] Brian C. Smith, (The Benzene Fingers,
The spectral properties of C6H6 and CCl4 shows
Part II: Let Your Fingers Do the Walking
similarity, in activities of the vibrational
Through
transitions, where each fundamental band of
the
Benzene
Fingers),
(Spectroscopy), Vol.31, (2016) No. 9, 30â&#x20AC;&#x201C;
both molecules is either IR or Raman active.
33.
However, the electronic spectral properties
[9] F.Carey " Organic Chemistry" Mc-Graw
show an Ď&#x20AC;â&#x2020;&#x2019;Ď&#x20AC;* electronic transition band for
Hill (2006).
C6H6 molecule, while it shows Ď&#x192;â&#x2020;&#x2019;Ď&#x192; * band for
[10] Brian C. Smith, (The Benzene Fingers,
CCl4 molecule.
Part I: Overtone and Combination Bands), (Spectroscopy), Vol.31, (2016) References
No. 9, 30â&#x20AC;&#x201C;33). [11] Th.
[1] G.Herzberg , (Infrared and Raman
Gomti Devi, A. Das, K. Kumar,
Spectra) Van Nastrand Reinhold Co.
(Anisotropy
shift
and
(1945).
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benzene
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(Spectrochim.Acta)
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[2] M.R.Mohammed and (Spectroscopic
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Interpretation
[3] Kamal Kayed, (The correlation between
Smith,
Raman carbonyl
chloro
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benz 60A
Spectral
Workshop),
carbon tetrachloride Raman spectra and
(Spectroscopy), Vol. 30, (2015) No. 1,
methanol configuration in CH3OH /CCl4
30â&#x20AC;&#x201C;33). [13] V. Talrose, E.B. Stern, A.A. Goncharova,
mixtures), (Chemtech Research), Vol.8,
N.A. Messineva, N.V. Trusova, M.V.
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Isotopic
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[15] M.lto, T.Shigeoka, (Raman spectra of benzene
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benzene-d6
[23] N. Rontu Carlon, D. K. Papanastasiou, E.
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(Spectrochimica Acta), Vol.22,(1966),
Newman, and J. B. Burkholder, (UV
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[16] Jong Chan Lee, Dong Eun Lee and Thomas
oxide (N2O) and carbontetrachloride
Schultz,
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rotational
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Raman
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benzene),
atmospheric
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[17] Dimitri MARCHAND, (In situ detection benzene
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