AL-KUT UNIVERSITY COLLEGE FOR SCIENTIFIC AND APPLIED SPECIALIZATIONS

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‫مجلة كلية الكوت الجامعة‬

REFEREED SCIENTIFIC AND ACADEMIC JOURNAL PUBLISHED BY CENTER OF RESEARCH, STUDIES AND PUBLICATIONS AL-KUT UNIVERSITY COLLEGE

FOR SCIENTIFIC AND APPLIED SPECIALIZATIONS Chairman of Board-President of the Foundation Commission Dr. Talib Zedan Al Musawi

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Chief in Editor

Managing Editor

Assist. Prof. Dr. Ahlam Hussien Al Musawi

Assist. Prof. Dr. Natiq Abdullah Ali

Editorial Board Prof. Dr. Sharov Vadim Ivanovich

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

Prof. Dr. Mohammed Abdulwahhab Munshid Prof. Dr. Ahab mohammed hussain Prof. Dr. Adawih Jemaah Hiader

Prof. Dr. Nassir Mohammed Fahad

Prof. Dr. Hafid mohammed dhuyab Prof. Dr. Ali hussain rishak

Assist. Prof. Dr. Nadiah Hashim Al-Noor Dr. Talib Zedan Al-Musawi Dr. Rabi Nori

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

Scientific and Linguistic Supervision

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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

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29-37

Rabi, Dr. Talib and Esam – Design and Construction ……

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K.U.C.J

Pages 1-8

Vol. 4 Issue 2 2019 4th Year

‫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

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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 380m 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.

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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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‫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

Nagham and Talib – Study the Optical …….

K.U.C.J

Vol. 4 Issue 2 2019 4th Year

Pages 9-17

‫( 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

K.U.C.J

Nagham and Talib – Study the Optical …….

Vol. 4 Issue 2 2019 4th Year

Pages 9-17

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

K.U.C.J

Nagham and Talib – Study the Optical …….

Vol. 4 Issue 2 2019 4th Year

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

K.U.C.J

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Vol. 4 Issue 2 2019 4th Year

Pages 9-17

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

K.U.C.J

Nagham and Talib – Study the Optical …….

Vol. 4 Issue 2 2019 4th Year

Pages 9-17

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

Nagham and Talib – Study the Optical …….

K.U.C.J

Vol. 4 Issue 2 2019 4th Year

Pages 9-17

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

Nagham and Talib – Study the Optical …….

K.U.C.J

Vol. 4 Issue 2 2019 4th Year

Pages 9-17

(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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K.U.C.J

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

K.U.C.J

Meriam â&#x20AC;&#x201C; Comparison of Antibacterial â&#x20AC;Śâ&#x20AC;Ś.

Vol. 4 Issue 2 2019 4th Year

Pages 18-28

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

K.U.C.J

Meriam – Comparison of Antibacterial …….

Vol. 4 Issue 2 2019 4th Year

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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Meriam â&#x20AC;&#x201C; Comparison of Antibacterial â&#x20AC;Śâ&#x20AC;Ś.

Vol. 4 Issue 2 2019 4th Year

Pages 18-28

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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Meriam – Comparison of Antibacterial …….

Vol. 4 Issue 2 2019 4th Year

Pages 18-28

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

Meriam – Comparison of Antibacterial …….

Vol. 4 Issue 2 2019 4th Year

Pages 18-28

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

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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

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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).

bandwidth

studies

in

containing

molecule

benzene

aldehyde),

(Spectrochim.Acta)

molecular), (University Engineering and

(2004)211.

[2] M.R.Mohammed and (Spectroscopic

liqa'a A.Hammed,

study

of

[12]

Techniques). Vol.28, No.1, (2010),33-36.

Brian

C.

Interpretation

[3] Kamal Kayed, (The correlation between

Smith,

Raman carbonyl

chloro

(IR

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.

No.10 , 2015 ,pp 187-193.

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Efimkina, The NIST WebBook, CAS:

CCl4 v1 Mode: Theoretical Prediction of

108-95-2, (10-12-2012).

Isotopic

[14] Howard Mark, Mike Bradley, (Review of

Effects),

(J.

Chem.

Educ).2015,92,6,1081-1085

New Spectroscopic Instrumentation for

[22] W. M. Haynes, editor-in-chief London.

2018), (Spectroscopy), Vol.33, (2018)

Handbook of Chemistry and Physics (95th

No.5, 28–50).

edn), CRC Press, 2014.

[15] M.lto, T.Shigeoka, (Raman spectra of benzene

and

benzene-d6

[23] N. Rontu Carlon, D. K. Papanastasiou, E.

crystals),

L. Fleming, C. H. Jackman, P. A.

(Spectrochimica Acta), Vol.22,(1966),

Newman, and J. B. Burkholder, (UV

No.6, 1029–1044).

absorption cross sections of nitrous

[16] Jong Chan Lee, Dong Eun Lee and Thomas

oxide (N2O) and carbontetrachloride

Schultz,

(High-resolution

rotational

(CCl4) between 210 and 350K and the

Raman

spectroscopy

benzene),

atmospheric

of

(Physical Chemistry Chemical Physics),

[17] Dimitri MARCHAND, (In situ detection benzene

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UV

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[18] V. Talrose, E.B. Stern, A.A. Goncharova, N.A. Messineva, N.V. Trusova, M.V. Efimkina, The NIST WebBook, CAS: 7143-2, (10-12-2012).

[19] V. Talrose, E.B. Stern, A.A. Goncharova, N.A. Messineva, N.V. Trusova, M.V. Efimkina, The NIST WebBook, CAS: 110-82-7 (10-12-2012).

[20] James D. Gaynor,a,b Anna M. Wetterer,a Edward J. Valentea and Steven G. Mayer, (The ν3ν4 difference band contribution to the CCl4 symmetric stretch (ν1) mode),(

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