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K.U.C.J Al-Kut University College Journal

Refereed Scientific Journal Published by Center of Research, Studies and Publication

Kut University College

Chairman of Board President of the Foundation Commission

Dr. Talib Zedan Al-Musawi

Chief Editor

Managing Editor

Asst.Prof. Dr. Ahmed Sabeeh Attiya

Asst.Prof.

Dr.

Ahlam Hussien Al-Musawi

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Asst.Prof. Dr. Sharov Vadim Ivanovich–Biology(Russia) Prof.

Dr. Sklyarenko Semen Alexandrovich- (Moscow,Russia)

Prof.

Dr.

Marei

M.

El-Ajaily

(Libya)

Prof.Dr.

Nabil

Mohie

Abde l-Hamid

(Egypt)

Prof.Dr.

Mahmoud

Ahmed

Souror

(Lebanon)

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Dr.Lutfy

Hameed

Jodat

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economy(Iraq)

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Taghreed

Hashim

Al-Noor

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Chemists (Iraq)

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Jamal

Al-Haidary

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Dr.

Khathir

Mahdi

Amran

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Dr.

Mohammed

Saleh

Mahdi

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Laser

Eng.(Iraq)

Prof.

Dr.

Phakher

Jaber

Mater

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Quran

Science

(Iraq)

Prof.

Dr.

Kadihm

Kareem

Al-Jabberi -Psychology (Iraq)

Prof.

Dr.

Mohammed

Abdulwahhab

Munshid–Laser

Eng.

Sheikh

Dr.

Salman

Al-Bahadly

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Quran

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(Iraq)

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Dr.

Adawih

Jemaah

Hider–Laser

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Scientific and linguistic supervision

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Lecturer Dr. Mohammed Anad Hussein

Lecturer Dr. Ahmed Shihab Hamed

Lecturer Dr. Badriah Nasser Abd Saeed

Asst.Lecturer Suheir Kareem Romani

Asst.Lecturer Yussra Challoob Madlool

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Asst.Lecturer Marwah Kareem Qasim

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Mohammed khalid abbood

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Prof. Dr. Ali Abdul Hussein Zoien Muntaha Raheem Meften

Special Issue/ The First International Scientific Conference No: One 29 - 30 April 2017Al Kut University College

Asst .Prof.Dr . Shmal Abdullah Al - Muffti

Asst .Prof.Dr . Shalal Abd Khamees Al -Robaiy

Asst.Prof.

i

K.U.C.J

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Al- Kut University College JournalThe Proceedings of First International Scientific Conference

ii

Issue One

mailto:[email protected]


http://www.alkutcollege.com/

Content of First IssueFirst International Scientific Conference

Al-Kut University College

1. Ownership Structure And Board Composition And Voluntary Disclosure LinkedWith Firm PerformanceDr. Hadi kadhim Attar …………………………………………………………..… 1

2. Isolation and detection of multidrug resistant e. coli from clinical Isolates ofinfected female urine samplesRami Mohaned Mahdi and Niyaf Nidhal Kadhem ……………………………….. 15

3. Design and construction of Optically intelligent system to monitor soil moistureto control the operations of irrigation of agricultural land.Dhafir A. Dhahir, Bushra R . Mahdi , Ahmed A. Hmad, ………………………..Naser M.Hadi , and Ahmed K. Ibrahim

26

4. Extraction of Lanthanum (III) Complex Coupled with SpectrophotometricMethod for Determination in Different SamplesSahar A.Hussein , Taghreed H. Al-Noor and R. K. Al-Kubaisy………………… 33

5. Characterization Of Zno /Cuo Nano Composite Preparation By ThermalChemical Spray Pyrolysis As Ammonia Gas SensingMahdi M. Mutter and Amel D. Hussan ………………………………………….. 45

6. Preparation of Some (Transition Metal-Flavylium Salt- Substitutes Chalcon)ComplexesOmar H. Al-Obaidi, Mohammad M. Al-Abid, Najat J. Al-Obaidi ……………... 52

7. Socio-economic Status impact on hypertension at Al- Zahra hospital in kut citySameeha Naser Abed ……………………………………………………… 61

8. Study of electrical characteristics of PS/Si heterojunction prepared by photo-electrochemical etching.Ayad Zwayen Mohammed ………………………………………………….. 73

9. Effect Of Continuous Wave Laser Diode Light–Curing On The Thermal Expansion OfNano-Composite Resin.Thoalfiqar Ali Zaher, Muna Youhana Slewa, Hanaa Nafee.Azeez ……………… 80

10. A feasibility study of PV - battery- fuel cell hybrid energy system for rural eMohammed Ridha Saeed Alhendawi, and Ali Saleh Aziz …………………………. 94

iii

First International Scientific Conference 29 – 30 April 2017 2017نیسان 30 – 29المؤتمر العلمي الدولي األول / ISSN: 2414 - 7419 Al-Kut University College/ Issue One كلیة الكوت الجامعة / العدد األول

OWNERSHIP STRUCTURE AND BOARD COMPOSITION AND VOLUNTARY DISCLOSURE LINKED WITH FIRM PERFORMANCE

Dr. Hadi kadhim Attar Management and Economics / University of Wasit

المستخلص

كمؤشر على أداء الشركة، استنادا إلى یعتقد بعض الباحثین أن الكشف الطوعي قد یمكن استخدامھ

ألصحاب المصلحة في جوانب عدیدة، واالداء العام إظھار األداء المالي ترغب شركات ان ال، مفادھا فكرة

جمھور، وبالتالي فإن للكون بما فیھ الكفایة للشركة لتظھر أدائھا یفي بعض الحاالت أن الكشف اإللزامي ال

االتجاه إلى الكشف عن المعلومات یطرح نفسھ طواعیة ویصبح الالزمة. من ناحیة أخرى، الكشف الطوعي

یمكن أن تؤخذ سلبا من جھة نظر األداء في الشركات التي انخفاض األداء قد یحاولون إخفاء ضعف األداء

العام من خالل توفیر معلومات إضافیة عن شركاتھم للجمھور، والتي المستخدم من التقاریر المالیة المالي أو

سیكون لدیك فكرة أن یقول لھ / لھا، أنھ إذا كان ھذا الشركة لیست أداء جیدا جدا انھا لن تكشف المعلومات

الرئیسیة لحوكمة الشركات مثل ومع ذلك، جادل العدید من الدراسات أن ھناك عالقة بین الصفات . طواعیة

ھیكل الملكیة وتكوین المجلس ومدى الكشف الطوعي. ھیكل الملكیة وتكوین مجلس على وجھ الخصوص،

فقد كان معروفا كأحد العوامل التي تؤثر على اإلفصاح الطوعي. وقد أجریت العدید من الدراسات حول العالقة

. خرابین حوكمة الشركات واإلفصاح الطوعي خارج مؤ

Abstract

Some researchers believe that voluntary disclosure may can be used as an

indicator on the firm’s performance, based on the idea that says, companies

like to show their high financial and general performance to the stakeholders in

many aspects, in some cases mandatory disclosure would not be enough and

sufficient for the company to show their performance the public, therefore the

trend to disclose information voluntarily arises and becomes necessary. On the

other hand, voluntary disclosure can be taken negatively from performance

point of view in which low performance companies may try to hide their poor

financial or general performance by providing extra information about their

company to the public, in which the user of the financial reports will have the

idea that tells him/her, that if this company is not performing very well it would

not disclose information voluntarily. However, numerous studies have argued

that there is a relationship between major corporate governance attributes such

as ownership structure and board composition and the extent of voluntary

disclosure. Ownership structure and board composition in particular, have

been known as one of the factors that affect voluntary disclosure. Numerous

1


studies on the relationship between corporate governance and voluntary

disclosure have been carried out recently.

PART ONE

1.0 Introduction

According to Chobpichie, (2008) voluntary disclosure is the external

reporting done beyond what is mandated. It covers all data which concerns both

subsidiaries and the group itself. However, the increasing amount of voluntary

disclosure among firms all over the world have motivated the researchers in this

particular area to wonder and explore factors that could make the firm to disclose

information that it is not mandated to disclose it in the first place.

Over years, corporations have had to disclose certain information regarding

the company’s financial position, management, creditors, competitors, and

shareholders. This type of disclosure is considered as a mandatory disclosure,

meaning that corporation must disclose certain information.

Giacomo Boesso (2007) argues that, in recent years dissatisfaction with

corporate mandatory disclosure has led the investors, financial markets and other

key stakeholders to demand that companies voluntarily provide more comprehensive

information about their long-term strategies and performance. This dissatisfaction

with the quality and the effectiveness of financial reporting has also received

worldwide attention from the academics. However, demand for enhanced

disclosures has been further fuelled by the increasing popularity of the stakeholder

approach that has resulted in a widespread realization that the interactions of a

company are not limited to just shareholders. There are other stakeholder groups as

well, who also have a right to be provided with information about how the activities

of the company impact them. Thus, the dissatisfaction with mandatory disclosures

and the demand for increased stakeholder reporting have led to initiatives in

practically every part of the world, and have encouraged companies to improve

stakeholder reporting.

According to the discussion above, it can be argued that voluntary disclosure

is one of the important things that have an importance for both, the firm and its

2


stakeholders as well, in the way that motivates researchers, students, and academics

to study the drivers, determinants, the impact, and the extent of voluntary disclosure.

Some researchers believe that voluntary disclosure may can be used as an

indicator on the firm’s performance, based on the idea that says, companies like to

show their high financial and general performance to the stakeholders in many

aspects, in some cases mandatory disclosure would not be enough and sufficient for

the company to show their performance the public, therefore the trend to disclose

information voluntarily arises and becomes necessary. On the other hand, voluntary

disclosure can be taken negatively from performance point of view in which low

performance companies may try to hide their poor financial or general performance

by providing extra information about their company to the public, in which the user

of the financial reports will have the idea that tells him/her, that if this company is

not performing very well it would not disclose information voluntarily.

However, numerous studies have argued that there is a relationship between major

corporate governance attributes such as ownership structure and board composition

and the extent of voluntary disclosure. Ownership structure and board composition

in particular, have been known as one of the factors that affect voluntary disclosure.

Numerous studies on the relationship between corporate governance and voluntary

disclosure have been carried out recently.

1.1 Problem statement

Over a long time, it is known that a corporation must disclose certain information

about itself. On the other hand, studies on the issue have shown that all mandatory

disclosure is no more satisfying for the corporation’s stakeholders, which means that

some individuals, institutions, and governments are not satisfied with the

information provided by the corporations mandatorily. Therefore, corporations have

started to provide some extra information in order to fill the gap that is represented

by the dissatisfaction of the typical mandatory disclosure.

Recently, voluntary disclosure has become one of the important issues that

researchers consider worth studying. However, numerous studies have been done in

this particular area to examine the relationship between corporate governance

attributes and voluntary disclosure. Studies in on corporate voluntary disclosure

3


have been carried out in both developed and developing countries. Such studies

similar to the one that has been done by Eng and mak (2003) suggests that corporate

governance plays an important role in determining the extent of corporate voluntary

disclosure assuming that corporate ownership structure and board composition can

affect the voluntary disclosure.

However, companies may voluntarily disclose some information about their

financial, non financial or strategic information, though this can still be poorly

performing and using this kind of action to cover or hide their business failure. On

the other hand, some companies might be using voluntary disclosure to show the

stakeholders how successful the firm is based on facts and true figures. However, a

current study might be attempting to find the main drivers of this voluntary

disclosure in terms of performance as well as ownership structure and other

corporate governance attributes.

Chau, et al., (2002), Patton, et al., (2004), Ghazali (2006) and many other

researchers caution that their results on the relationship between corporate

governance attributes and voluntary disclosure cannot be generalized, in other

words, what applies of this relationship in one country might not be applicable for

another. Therefore, in order to further know if there is a relationship between these

corporate governance attributes and voluntary disclosure, the studies recommended

that this relationship is examined in that particular country by itself.

Apart of the numerous studies that have been done on this relationship in

developed and developing countries, studies on the corporate voluntary disclosure in

general and on the relationship between corporate governance and voluntary

disclosure in particular, are few in the Malaysian market considering that Malaysia

is a developing country with an emerging capital market, and the fact that many

corporations in Malaysia are either family or government owned corporations.

Therefore, this study is carried out to add impetus on this issue in the Malaysia

market, and furthermore to benefit corporations and stakeholders in Malaysia by

examining the relationship between the firms’ corporate governance and their

voluntary disclosure.

1.2 Research Objectives

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The main objective to explore the relationships between corporate

governance attributes (ownership structure and board composition) and corporate

voluntary disclosure, controlling for firm size and leverage in the Malaysian listed

companies for the year 2009. Specifically this study aims to:

1. To examine if there is a significant relationship between ownership

structure and voluntary disclosure and what relationship between this disclosure and

firm performance in the Malaysian listed companies for the year 2009 through the

following:

a) To examine if there is a significant relationship between managerial

ownership and voluntary disclosure and what relationship between this disclosure

and firm performance in the Malaysian listed companies for the year 2009.

b) To examine if there is a significant relationship between government



c) To examine if there is a significant relationship between block holder



2. To examine if there is a significant relationship between board composition (represented by independent directors) and voluntary disclosure and what relationship between this disclosure and firm performance in the Malaysian listed companies for the year 2009.

PART TWO

LITERATURE REVIEW 2.0 Introduction This section provides discussions on corporate governance, voluntary

disclosure, followed by reviews on corporate governance attributes and their

influence on voluntary disclosure. Various empirical studies are also reviewed to

provide a better understanding on the relationship between that corporate

governance attributes influence on voluntary disclosure.

2.1 Agency Theory and Voluntary Disclosure

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The agency theory suggests that disclosure vary with quotations status in

which there is a detachment of ownership from management. The agency costs

might arise because of conflicts between either, shareholders and managers, or

between bondholders and shareholders’ managers. However, the problem here is

that the agent is likely to have access to some important information than the

principle, in a situation known as information asymmetry. Therefore, as long as it is

hard for the principle to notice the managers’ behaviours, it is likely for the

managers to take an advantage of these superior information.

Hanifa and Rashid (2004) However, corporation nowadays have adopted

various michanesm such as voluntary disclosure trying to alleviate the adverse effect

of information asymmetry. Hanifaand Rashid (2004) find that, as larger is the firm

are as the variety of the stockholders increases, which increases the agency cost in

the firm, thus, larger firm are expected to voluntarily disclose more than smaller

firms in order to reduce the agency cost.

2.2 Voluntary Disclosures

Matoussi, et al. (2007) suggests that voluntary disclosure is a game of

contradictory powers (motivating forces, and dissuasive forces). The process of

voluntary disclosure results thus from an arbitration between the economy of costs

(agency costs, political, capital) that this publication can procure to the company,

and the generation of costs (direct and indirect) as a result of this publication.

Peterschuster, et al, (2006) note that the contemporary phenomenon of

market globalization has led companies to become more international in their trends

and has also led business environment to have more complexity. While capital

markets now offer un-forecasted investment opportunities, as a consequence resulted

from these trends is the tendency for investors to be confronted with a redundancy of

information about uncountable corporate activities. In addition to making the

required compulsory disclosures, more and more companies are disclosing

information on a voluntary basis, presumably in the hopes that this extra data will

fasten the stock market to recognize hidden elements of corporate value.

Einhorn (2007) states that economists believe that sellers offering assets for

sale are encouraged by the market to fully disclose to potential buyers any single

relevant private information. He also points out that the immense research in

6


providing an understanding of corporate voluntary disclosure strategies has

primarily focused at explaining why firms do not fully disclose their private

information in capital markets. Following a variety of theories that explain the

covering of information, Einhorn (2007) highlights the uncertainty of investors

about the reporting objective of managers as another explanation.

Kristandl et al., (2007) argue that voluntary disclosure of decision-useful

corporate information is considered to be the first step in solving the alleged

problems of traditional financial reporting. Furthermore, they argue that the well-

defined objectives of voluntary disclosure can narrow the gap between the

company’s potential market value and its current market value.

2.3 Corporate Governance Attributes and Voluntary Disclosure

Numerous studies have been done to examine the relationship between

corporate governance and corporate voluntary disclosure. Following is a review for

some of the relevant studies that are done in the past.

Noting that corporate governance involves various activities that can reduce

agency cost, Baek, et al. (2009) investigate the impact of managerial ownership on

disclosure quality in US listed firms, the study reveals that higher managerial

ownership is associated with higher levels of and quality of disclosure in general.

Matoussi et al. (2007) studied the relationship between ownership structure

and voluntary disclosure in annual reports of Tunisian listed firms using panel data

for the years 2003 to 2005, excluding financial firms. Their study reveals that the

level of voluntary disclosure tends to increase over time. Furthermore, the study

shows that managerial ownership and a good quality of corporate governance are

positively correlated to the voluntary disclosure. However, the dependent variable

(voluntary disclosure) was proxied by an un-weighted disclosure score was

developed by the researchers based on a developed checklist for the disclosure. All

the data required for their study were abstracted from the Tunisian non-financial

listed companies’ annual reports for the years 2003-2005.

Parallel study was carried out by Yuan and Xiao (2007) aimed at examining

the impact of ownership structure and board composition on the extent of voluntary

disclosure in China. The study of Yuan and Xiao (2007) uses ordinary least square

(OLS) regression for 559 Chinese listed companies in the year 2002. Yuan and Xiao

(2007) find that block holder ownership and foreign listed shares are positively

7


associated with voluntary disclosure, while managerial ownership, state ownership

appear to have no significant impact on voluntary disclosure.

Patton et al. (2004) examined the impact of ownership structure on the extent

of voluntary disclosure, on 50 non-financial Czech companies for the year 1993,

using cross sectional data extracted from Czech annual reports. The study reveals

that ownership structure is a significant determinent of the extent of corporate

voluntary disclosure. Furthermore it finds that block holder ownership is positively

related to the extent of voluntary disclosure in the newly privatized firms in Czech

republic.

However, much of the research to date has focused on developed countries.

Inadequate attention is dedicated to the voluntary financial disclosure of companies

in other countries, in China for example. Wang et al. (2008) examined empirically

the determinants of voluntary disclosure in the annual reports of Chinese listed firms

that issue both domestic and foreign shares. They find that the level of voluntary

disclosure is positively related to the proportion of state ownership, foreign

ownership. In addition, they conclude that voluntary disclosure or information

exceeds mandatory disclosure, considering that globalization of the world’s financial

markets has received large attention in the accounting literature recently.

Barako (2007) examines the association between corporate governance

attributes, ownership structure and company characteristics with voluntary

disclosure in the annual reports of Kenyan companies from 1992 to 2001. Barako’s

study uses panel data analysed using pooled Ordinary Least Square (OLS) with

Panel-Corrected Standard Errors (PCSEs) to estimate the determinants of voluntary

disclosure of various types of information. The results of the study indicate that,

disclosures of all types of information are influenced by corporate governance

attributes, ownership structure and corporate characteristics. Generally, there is

evidence that the level of voluntary disclosure was increasing in all categories over

time along with the study period.

In investigating the association between corporate governance structure and

the extent of voluntary disclosur, Boesso and Kumar (2007) proxy corporate

governance structure by the ratio of independent directors in the board to the total

8


number of directors. Boesso and Kumar (2007) find that proportion of independent

directors is not one of the voluntary disclosure extent determinants.

Chobpichien (2004) investigates whether the quality of board of directors

and ownership structure are significantly related to the voluntary disclosure index in

the annual reports of 317 non-financial companies listed on the Stock Exchange of

Thailand in 2004. The study finds that the quality of board of directors and the

ownership structure of the firm have a significant impact on the voluntary disclosure

index. The study reveals that the higher the board of directors’ quality, the higher is

the voluntary disclosure index. Board of director index has many dimensions,

proxied by chairman-CEO separation, proportion of independent non-executive

directors on the board, are significant factors associated with the voluntary

disclosure index. The above results show that the relationship between the quality of

board of directors and voluntary disclosure index will not necessarily be the same

between companies with major shareholder owners (positively and negatively

moderate).

Wong’s (2001) results indicate that the existence of an audit committee is

significantly and positively related to the extent of voluntary disclosure, while the

percentage of family members on the board is negatively related to the extent of

voluntary disclosure. The study provides empirical evidence to policy makers and

regulators in East Asia for implementing the two new board governance

requirements on audit committee and family control. The most significant

governance variable, percentage of family member on board, shows that the more

family members on the board, the less likely that a firm has a higher extent of

voluntary disclosure.

PART THREE

CONCLUSION

3.0 Personal Opinion and Conclusion

We have reviewed some previous studies that discuss the issue of the relationship

between performance and ownership structure and voluntary disclosure as well, the

finding of the studies do not indicate or tell us one conclusion or result about these

relationships, meaning that the relationships differs as the country examined,

industry chosen, and period of time changes.

9


For example, Imam, M. O, and Malik, M. provided an evidence the foreign

ownership along with block holder or institutional ownership are associated with

high firm performance, after examining the Bangladesh stock market excluding

financing firms for the year 2000 and 2003.

That gives us an indication that ownership structure is an important determinant of

firm performance.

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First International Scientific Conference 29 – 30 April 2017 2017نیسان 30 – 29لمؤتمر العلمي الدولي األول / ISSN: 2414 - 7419 Al-Kut University College/ Issue One كلیة الكوت الجامعة / العدد األول

Isolation and detection of multidrug resistant e. coli from clinical Isolates of infected female urine samples

Rami Mohaned Mahdi * ,Niyaf Nidhal Kadhem **

*Analysis pathology techniques department / Al- kut university ,** Biotechnology Research Center /Alnahrain Uni.

ABSTRACT

The present study deals with the isolation of E. coli from different clinical samples and its genetic diversity. The clinical samples were collected from a microbiology laboratory, Bangalore, India. The samples were pus, wound and blood. The isolates were identified by Gram's staining, biochemical characterization and by using selective media. The organisms isolated were E coli. The microorganism were grown overnight at 37 0 C in selective media such as, EMB agar. In this study, biochemical tests were done for the identification of E. coli stains. In the Indole test after addition of Kovac’s reagent the cherry red colour appeared indicating positive results.

1. Introduction

In Methyl Red test all the samples showed MR positive and in Voges Proskauer test all the tested samples showed VP negative. In citrate utilization test all the tubes showed the green colour after the incubation of 48 hours which indicated that the test organisms were citrate negative. In catalase test, after addition of hydrogen-peroxide there were bubble formation and in oxidase test, the freshly prepared solution tetramethyl-p-phenyl diamine dihydrochloride when added to samples, purple colour developed , indicating that the samples were oxidase positive. The other biochemical test results like urease test, nitrate reduction test, starch hydrolysis test and casein tests of the clinical isolates gave the expected results for E. coli. This was a confirmation that the isolates were indeed E. coli. Antibiotic sensitivity tests of the E. coli samples were then performed to check for their susceptibiltity against few specific antibiotics like gentamicin (GM) 10µg, ciprofloxacin (CIP) 5µg, ceftriaxone (CRO) 30µg, ampicillin (AMP) 10µg, and co-trimoxazole (SXT) 25µg. Majority of the E. coli isolates exhibited resistance to ampicillin while a few test organisms showed intermediate and sensitive respectively. Co-trimoxazole antibiotic sensitivity test of the isolates showed that they were resistant while some exhibited intermediate and sensitive responses respectively. E. coli isolates were mostly resistant to gentamicin, ciprofloxacin and ceftriaxone while few

15

First International Scientific Conference 29 – 30 April 2017 2017نیسان 30 – 29لمؤتمر العلمي الدولي األول /

ISSN: 2414 - 7419 Al-Kut University College/ Issue One كلیة الكوت الجامعة / العدد األول

of the isolates gave intermediate responses. Most isolates (80.4%) exhibited multi-drug resistance.

2. Methods and materials:

isolate and diagnose the bacteria of E.cloi from urine samples form more than twenty women were suffering from chronic urinary tract infection using the EMB agar and biochemical tests

3. Results and Discussion

Antibiotic Sensitivity test

The Kirby-Bauer Disc Diffusion Method (Struve et al, 2003) was used to test the in vitro susceptibility of the identified isolates to gentamicin (GM) 10µg, ciprofloxacin (CIP) 5µg, ceftriaxone (CRO) 30µg, ampicillin (AMP) 10µg, and co-trimoxazole (SXT) 25µg. A sterile platinum loop was used to pick colonies of E. coli from the culture plate and emulsified in 4 ml of sterile peptone water to match with 0.5 McFarland turbidity standards (1.5x108 cfu/ml). Using a sterile swab, the surface of Mueller Hinton Agar (Oxoid, Basingstoke, UK) in a Petri dish was evenly inoculated with the suspension.

With the Petri dish lid in place, about 10 minutes was allowed for the surface of the agar to dry. A multichannel disc dispenser (Oxoid, Basingstoke, UK) was used to deposit the antibiotics discs onto the surface of the inoculated medium. The plate was then incubated at 37°C for 18 hours. The diameters of the zones of inhibition were measured in millimetres

Table 1:inhbtion zones.

Antibiotics Doses Inhibition zone by (mm)

S I R Ampicillin(10ug) ≥30 ≥ 11 ≤10

Cptrimoxazole(25ug) ≥17 ≥13 ≤12 Gentamicin(10ug) ≥21 ≥17 ≤16 Ciprofloxacoin(5ug) ≥26 ≥19 ≤18

Ceftriaxone(30ug) ≥19 ≥ 15 ≤14

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Table 2: Antibiotic Sensitivity test results.

Samples Ampicillin Gentamicin Cotrimaxanole Ciprofloxin Ceftriaxone

S1 R R R R R S2 R I R R R S3 R I R S R S4 R I R R I S5 R R R R I S6 I R I S R S7 I S S S R S8 I S S I S S9 S S S I S S10 R S I I R S11 R S R S R S12 R S R R R S13 R S R I R S14 R S R R R S15 R S R R S S16 R R R I I S17 R S R R I S18 R S R I I S19 R S R R S S20 R S R I I

According to Archibald (2004), extensive use of antibiotics creates selective advantage for microorganisms and that transmission of resistant strains from patient to patient within hospitals is possible. The bacteria studied in this project, E. coli, is an important bacteria commonly implicated in many nosocomial diseases (Archibald, 2004; Blanc et al, 1998; Kiffer et al, 2005; Shrestha, et al, 2009; Strateva et al, 2007). The presence of resistant strains of this organism in hospitals and environment should be of much concern because both patients and hospital staff are exposed to these microorganisms.

Jarvis and Martone reported that E. coli as themost common nosocomial pathogen in some hospitals in theUnited States. Also, E. coli has been reported to be among themost frequent isolates in hospitals in Ethiopia .Among the three hospitals from which the samples orswabs were taken, E. coli isolates were widely distributed invarious locations throughout the three hospitals for which samples were analyzed . By the number of Bio- chemical tests that proved the the type of bacteria that found in the urine samples of infected proved type of bacteria in it is the bacteria of E.coli , the laboratory results of tests that performed are identical what samples isolated from urinary tract infections give, as in Table 1. As well as tests showed sensitivity that have been made by 20 infected urine sample also showed the results in Table No. 2 and No. 3

17



Just been identified is the kind of anti-resistant and non-resistant and anti-bacteria, which has sensitive

By measuring the diameter area where there are no bacterial growth around the antibiotic disc and During the counting of samples sensitive and non-sensitive and medium resistance to antibiotics and make mathematical calculations by law, the percentage were the percentage of the conclusion of each antibiotic used in the sensitivity tests as shown in Table 4 and the drawing below Reached the following results, About 91% of the E. coli isolates exhibited resistance to ampicillin while 7% and 2%, respectively, showed intermediate and sensitive. For cotrimoxazole (trimethoprimsulphamethoxazole), 78.% of the isolates were resistant while 10 and 12% intermediate and sensitive responses. the E. coli isolates also showed resistance to gentamicin, ciprofloxacin, and ceftriaxone, the 26% and 46% , while 14 %, 30% and 20% gave intermediate responses. Ceftriaxone, ciprofloxacin, and gentamicin sensitive isolates were also give of 20 , 24% and 60% . The majority of the gentamicin sensitive E. coli isolates (28.9%) was isolated from the male wards followed by floor samples (21.1%). None of the drainage samples were resistant to gentamicin, while 20% each from the floor and female wards proved resistant. 26.9% isolates from bench samples exhibited intermediate response to gentamicin. Out of the total, 46 E. coli isolates exhibited intermediate response to ceftriaxone, 30% were from the male wards, 21.4% from floor and 2.2% from drainage samples. Most of the E. coli resistant isolates (26.9%) were from the benches and 19.2% from male wards while no resistant strains were recovered from door handles. Ciprofloxacin-resistant E. coli isolates were recovered from floor samples (29%) followed by the samples from pediatric wards (19.4%). E. coli isolates which exhibited intermediate response to ciprofloxacin (30%) were in the samples/swabs from the male ward and none from door handles. Majority of the E. coli sensitive isolates were from female wards (30.4%) followed by male and pediatric wards samples (17.4%). Floors and benches samples showed equal ciprofloxacin sensitive E. coli strains of 13%. The distributions of ampicillin resistant E. coli isolates were 22.7, 20.5, and 19.3% for male wards, floors, and benches.Most of the E. coli isolates (80.4%) exhibited multiple drug resistance and measures such as observation of proper personal hygiene by health staff and patients, use of effective disinfectants in reducing the possible pathogenic organisms in these hospitals, and so forth. These findings have therefore showed the need for the hospital management to be concerned about the potential of hospitalized patients becoming infected with some nosocomial infections, especially resistant strains of E. coli.

18



Table 3: ratio of resistance depend on 20 of samples that used.

4. Conclusion: 1. According to tests that did on bacteria in the urine with the same biochemical

characteristics that cause UTI diseases Bactria strain has. 2. The Bactria that in found in urine The same strain that causes urinary tract

infections 3. Acquired resistant bacteria as a result of overuse or misuse of antibiotics 4. Its has ability to withstand the Acidic environment in the urine 5. Different percentages be resistant against antibiotics for various kinds of

antibiotics according to the results of Sensitivity tests 6. Lower percentage of resistant formed by Bactria against Gentamicin (antibiotic )

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First International Scientific Conference 29 – 30 April 2017 2017نیسان 30 – 29المؤتمر العلمي الدولي األول /

ISSN: 2414 - 7419 Al-Kut University College/ Issue One لیة الكوت الجامعة / العدد األول

ذكیة لمراقبة رطوبة التربة للسیطرة على عملیات بصریة تصمیم وبناء منظومة الزراعیة . األراضيالسقي في ,احمد خلیل ابراھیماحمد عاصي ,د.نصیر مھدي ھادي ,ظافر عزیز الظاھر, د.بشرى رزوقي مھدي

العلوم والتكنلوجیا

الخالصة

أدتالزراعة ھي واحدة من القطاعات المؤثرة على الجماھیر ولھا عواقب مباشرة على نمو بلدنا . وقد المحاصیل وعالوة على ذلك إنتاجالطرق التقلیدیة للسقي الى فقدان عناصر التربة والري. مما اثر بشدة على

أدتفي الظروف البیئیة وما الى ذلك الموارد . وتوافر تغیرات البیئة أدارةوبسبب العدید من القضایا مثل نظام الري المقنن وقد تم تصمیم نظام تحكم الي للري لتسھیل التحكم التلقائي بكمیات المیاه إنشاءالحاجة الى

نقدم تصمیما للري االلي الذي من الخزانات الى الحقل او المحاصیل المحلیة في جمیع المواسم الزراعیة .جھاز إنشاءخدام اللیزر. یعمل النظام لقیاس محتوى الرطوبة في التربة ثم بصریة باست بإشارةیعمل

استشعار الرطوبة لنموذج المقاومة الكھربائیة للتربة. یتم وضع استشعار الرطوبة االلكترونیة داخل التربة بصریة عبر الجو الى أشارة وإرسالالكترونیة الى دائرة المرسل أشارةیرسل المتحسس لقیاس الرطوبة .

دائرة االستقبال . الطریقة المستخدمة ھي لمراقبة مستمرة لمستوى رطوبة التربة لتحدید مااذا كان ھناك إمداداتفرعیة وھي أنظمة أربعةویمكن تصنیف العمل في حاجة الى الري وكمیة المیاه الالزمة في التربة . م الفرعیة للضخ التي تشكل نظام التحكم االلي بالري .الطاقة ووحدة االستشعار ووحدة التحكم والنظ

النتائج ان نوع التربة تتطلب كمیات مختلفة من المیاه للري . وأظھرت

Design and construction of Optically intelligent system to monitor soil moisture to control the operations of irrigation of

agricultural land. Dhafir A.Dhahir, Bushra R .Mahdi ,Ahmed A.Hmad , Naser M.Hadi ,

Ahmed K.Ibrahim Abstract Agriculture is one of the influential sectors which affects the masses and has direct consequences towards the growth of our country. Conventional ways of watering have led to loss of soil nutrient, leaching, under/over irrigation, severely affecting the crop yield. Further, due to numerous issues such as resource management, availability of electricity, changes in environmental conditions, etc., a need for efficiently managed irrigation system is created. An automatic irrigation control system has been designed to facilitate the automatic supply of adequate of water from a reservoir to field or domestic crops in all agricultural seasons. We present a design for automated irrigation setup which operates optically signal by using laser. The system works to measure the moisture content in the soil . A moisture sensor was constructed to model the electrical resistance of the soil .The electronic moisture sensor is put inside soil to measure moisture. Sensor sends an electronic signal to the transmitter circuit and sent optical signal through the atmosphere to the receiver circuit . The method employed is to continuously monitor the soil moisture level to decide whether irrigation is needed, and how much water is needed in the soil. A pumping mechanism is used to deliver the needed amount of water to the soil. The work can be grouped into four subsystems namely; power supply, sensing unit, control unit and pumping subsystems which make up the automatic irrigation control system. The results obtained showed that sandy soils

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require less water than loamy soils and clay soils require the most water for irrigation. Keywords: Automation, irrigation, control, pumping, soil moisture

1. Introduction

Humidity and moisture – definitions and terminology The term moisture refers to the content of water in a liquid or solid due to absorption or adsorption, while the term humidity is reserved for the content of water vapor in gases. Absolute humidity refers to the density of water vapor, i.e. the mass of water vapor per unit volume of gas. Since this is the same measurement for atmospheric pressure, the term absolute humidity is generally not used. The most commonly used terminology for humidity measurement are expressed in terms of Relative Humidity (RH). RH is the ratio of the actual vapor pressure of air at a particular temperature, to the saturation vapor pressure at the same temperature. The value of RH expresses the vapor content as a percentage of the concentration required to cause the vapor saturation, that is, the formation of water droplets (dew) at that temperature. Humidity and moisture measurements can be made by employing a range of methods that either probe the fundamental properties of water vapour or use various transduction methods that provide humidity-related measurements. The humidity and moisture measurements range from simple schemes involving the expansion and contraction of materials such as human hair to much more advanced techniques, such as using a miniaturized electronic chip or recently, the utilization of optical fiber technology. Some humidity that are in use widely are illustrated in Fig(1). In this paper, the focus is mainly on the methods and performance of RH and moisture sensor utilizing the burgeoning technology that is based on optical signal.

Fig. 1. Some conventional hygrometers that are currently in use in industry [3].

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Irrigation has been used to assist in the growing of agricultural crops, maintenance of landscapes, and re-vegetation of disturbed soils in dry areas and during periods of inadequate rainfall. In crop production, irrigation helps in protecting plants against frost, suppressing weed growth in grain fields and preventing soil consolidation. The old method used for irrigation was the use of watering cans, water channels that have to be opened and closed manually or backpack sprinklers. In this case, a lot of water is wasted in the process [2]. There is need for improvement on the existing or old forms of irrigation. An automated irrigation system needs to be developed to optimize water use for agricultural crops [3]. An intelligent automatic irrigation system has to have all the components that autonomously monitor and control the level of water available to the plants without any failure or human intervention [4]. The intelligent system should perform the following functions: 1. continuously monitor the amount of soil water available to plants (this is usually achieved using a sensing system). 2. determine if watering is required for the plants based on the information obtained from monitoring the soil water content. 3. supply exact (or approximate) amount of water required for the plants. This will be enhanced by how well it achieves requirement 1. 4. discontinue the water supply when the required amount has been delivered to the plants. This feature is important as the amount of water available for the irrigation system is not infinite, therefore water management is paramount. The advantages of automatic irrigation to the plants include saving money, water, conservation of labour and overall convenience [5, 6, 7, and 8]. The water supply needed by the system to perform its irrigation function can be from any source, i.e. well, river, stream, pond, lagoon, etc. However, it is most desirable if a constant source of water is available to the system in order to ensure continuity of operation. The most preferred arrangement will be a water reservoir which is constantly maintained at full capacity or a large source of fresh water which remains continually available irrespective of variations in weather or climatic conditions.

There are about four categories of methods, according to [9], proposed for scheduling irrigation effectively: • Entirely empirical method and without any kind of on-going measurement • Method based on monitoring soil moisture • Method based on estimates of water use from weather data, and • Method based on tracking the condition of the crop usually referred to as crop water stress. The method of monitoring the soil moisture is employed in this project work. By this method, the amount of water applied to the agricultural products is minimized and it reduces crop production cost. Irrigation methods, according to [10, 11] are based on the following; the experience of the farmer,the soil properties and environmental conditions.

2. Methodology

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The automatic irrigation system was designed to continuously sense the moisture level of the soil. The system responds appropriately by watering the soil with the exact required amount of water and then shuts down the water supply when the required level of soil moisture is achieved. The block diagram of this system is shown in fig(2).

Fig(2) the block diagram of the automatic irrigation.

3. The sensing element The moisture sensors were designed using probes made from corrosion-resistant material which can be stuck into soil sample. Voltage levels corresponding to the wet and dry states of the soil sample were computed by measuring the resistance between the moisture detector probes and matching them to output voltages of a comparator circuit. The sensor designed was made up of two conducting Aluminum metal probes connected with two terminal . The distance of separation of the probes was 4cm. The probes had conducting wires attached to them at the end above the block.

4. The pump A 220 V Ac -powered motor was used in designing the pump. The motor running circuit is an optical sensor that receives the light signal and turns it into an electric signal to operate the relay switch which in turn connects the alternating voltage to the motor.

5. The control circuit One of the most important components of an automatic irrigation system is the

irrigation controller also called a timer or clock [12]. A 555 timer was used as the brain of the control circuit due to its operational characteristics in the switching

29



mode. The circuit diagram is shown in fig ( 3 ).

Fig(3) The circuit diagram of motor operation

6. The power supply circuit A step-down transformer was selected to transform the 240V mains supply voltage to 15V for the power supply. The 15 V ac was converted to dc voltage using a full wave rectifier circuit.

7. Transmitter This circuit is used to drive the laser source at wavelength 532 nm at the power equal 10mw .

8. Receiver This part of system is used to detect the optical signal and convert it to electrical signal than amplify it . Electrical signal normally-open relay was used as the actuator to implement the triggering of the pump-motor circuit.

9. Circuit implementation The implementation of the electronic circuitry involved the computerized simulation of the system design, physical simulation of the circuit using a breadboard to ensure proper operation and the final implementation of the circuit on a Vero board. The system tested the presence of dry and wet soil and showed the system's efficiency in the operation of the motor for a limited time depending on the degree of wetness and soil. The photograph picture of irrigation system is shown in fig (4).

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Fig(4) The photograph picture of irrigation system

10. Conclusion Automatic irrigation control system has been designed and constructed. The prototype of the system worked according to specification and quite satisfactorily. The system components are readily available, relatively affordable and they operate quite reliably. The system helps to eliminate the stress of manual irrigation and irrigation control while at the same time conserving the available water supply. Improving Irrigation efficiency can contribute greatly to reducing production costs of agricultural products, thereby making the industry to be more competitive and sustainable. Reference [1] Abhinav Rajpal, Sumit Jain, Nistha Khare and Anil Kumar Shukla “Microcontroller-based Automatic Irrigation System with Moisture Sensor” Proceedings of the International Conference on Science and Engineering (ICSE 2011). [2] J. Green, I. Dyer, Measurement of humidity, Anaesthesia and Intensive Care Medicine 10 (2009) 45–47.

[3] Z. Chen, C. Lu, Humidity sensors: a review of materials and mechanisms, Sensor Letters 3 (2005) 274–295. [4] A. Monti, A. Zatta, Root distribution and soil moisture retrieval in perennial and annual energy crops in Northern Italy, Agriculture,

Ecosystems and Environment 132 (2009) 252–259. [5] A.D. Mackay, S.A. Barber, Soil moisture effect on root growth and

phosphorus uptake by corn, Agronomy Journal 77 (1985) 519–523. [6]- T.L. Yeo, T. Sun, K.T.V. Grattan, Fibre-optic sensor technologies for humidity and moisture measurement, Sensors and Actuators A 144,(2008) 280–295.

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[7] -J.M. Corres, F.J. Arregui, I.R. Matias, Sensitivity optimization of tapered optical fiber humidity sensors by means of tuning the thickness of nanostructured

sensitive coatings, Sensors and Actuators B 122 (2007) 442–449.

[8]. Karthikeswari M, Mithraderi P “Automated Irrigation System in Agriculture using wireless Sensor Technology” International journal of Advanced research in Electrical,Electronics and Instrumentation Engineering Vol.3, issue 12, December 2014 ,p. 13622-13627. [9]. Liai Gao, Meng Zhang, Geng Chen “An Intelligent Irrigation System based on wireless Sensor Network and Fuzzy control”Journal of Networks, Vol. 8, No 5, 2013 p. 1080-1087 [10]. Suraj S. Avatade, Dhanure S.P “Irrigation System Using wireless Sensor network and GPRS” International Journal of Advance Research in Computer and Communication Engineering. Vol.4, issue 4, May 2015 p.521-524. [11]. Rahim Khan, Ihsan Ali, M.Asif Suryani, Mushtag Ahmad and Muhammad Zakarya “ Wireless sensor Network based Irrigation Management System for Container Grown Crops in Pakistan” World Applied Science Journal 24(8),2013 p.1111- 1118. [12]. Purnima, SRN, Reddy “Design of a remote monitoring and control System with Automatic Irrigation System using GSM blue-tooth” International Journal of Computer Applications Vol. 47 No 12, June 2012.

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Extraction of Lanthanum (III) Complex Coupled with Spectrophotometric Method for Determination in Different

Samples

Sahar A.Hussein* , ** Taghreed H. Al-Noor and R. K. Al-Kubaisy ** *faculty of Pharmacy, University of kufa**.Chemistry Department-College of

Education for Pure Science-Ibn Al-Haitham Baghdad University [email protected] ** [email protected],

Abstract:- 2- [(4-Benzyloxy phenyl)azo] -5-nitro-4-phenyl imidazol (BANI) used as complexation agent to form ion association complex. pH=11, which is giving higher absorbance at λmax= 501 nm , in presence of 80 μg La(III) in 5mL and 1×10-4 M of [BANI], this study show ion pair complex extracted have a structure [1:1],[M];[L] and thermodynamic study show extraction method of La(III) was exothermic with thermodynamic data ΔHex=-0.067 KJ/mol, ΔGex-52.87321 KJ.mol-1 and ΔSex= 190.191 J.mol-1K-1as well as this research contain another studies and synergistic effect study. From other hand used this method and organic reagent for spectrophotometric determination of La(III) of different samples

Key word: Cerium(ΙΙ) , Solvent extraction , 4- [N-(5-methyl isoxazol-3-yl)benezen sulfonamide azo]-1- Naphthol.

1. Introduction Solvent extraction of Lanthanum (III) by Di-(2-ethylhexyl)phosphoric acid from

chloride solution in the presence of (Lactic acid) as complexing agent. The active separation parameters can be completed when the Lactic acid is added to the aqueous solution of the extraction system. The Lactic acid can be effectively recycled using (TBP) as extractant, by the use of a counter current extraction process, which recognize the emission standards of contaminated from rare earths manufacture. so the environment-friendly and simple complexing method has been proved to be an active strategy for separating light rare earths, and supply a positive effect on the purification of lanthanum(III) [1]. Extraction ability of 8-HQ in countenance of DB18C6, DCH18C6 , and DBP18C6 crown ethers for chosen Ln(III) ions from acidic media to DMSO/chloroform solvent system. The study effect of HNO3 concentrations on selectivity of extraction, the effects of solvent, pH, Crown ether organic reagent and concentrations of crown ethers have been investigated. The crown ether DCH18C6 shows high separation ability for Lanthanide (III) ions for optimum concentration 5µM at (pH 3.8) from strong acidic media with 8-HQ as comparison to original 18C6 and other derivatives [2] . Liquid –liquid extraction of aqueous La3+ picrate with 18-Crown-6, dibenzo-18-Crown-6, benzo-15-Crown-5, dibenzo-24-Crown-8 and dicyclohexyl-18-Crown-6 dissolved in 1,2-Dichloroethane and other organic solvents. The La3+ cation is extracted as [2:1] [L:M] sandwich complex with B224C8 while as [1:1]complex with 18C6, B218C6, B15C5 and Cy218C6. The impact of different variables on the

33

mailto:[email protected],%20%20%20**%20%[email protected]

mailto:[email protected],%20%20%20**%20%[email protected]


D-value of Lanthanum (ІІІ) such as organic solvents and time of equilibrium. The measurements are made by using differential pulse polarography and direct current polarography, using (0.1M,KCl) as supporting electrolyte[3]. Synthesized and characterized of N, N-dibutyldiglycol amic acid (HLI) as well as N, N-dioctyldiglycolamic acid (HLII) by conventional spectroscopic methods. The analysis of the extraction equilibria revealed that the extracted species of lanthanum and europium ions by both of the extractants had a 1:3 metal to ligand ratio. Regardless to the diluent used, the order of selectivity presented by the investigated extractants was Er(III)>Eu(III)>La(III). It is noteworthy that, a significant enhancement in separation of the studied rare earths by the extractants was achieved in their competitive extraction experiments with respect to that obtained in single component extraction experiments [4].

2. Apparatus Spectrophotometric measurements used double beam (Uv.-Vis.),(Japan), pH

measurement carried out by pH –meter , WTW CE ,E163694, (Germany). As well as for studied the structure of organic reagent prepared used FT-IR 8400 S(CE), Shimadzu corporation. Element analysis Carried out by Micro analytical unit, 1108 C.H.N elemental analysis.

Reagents 3. Materials and Solutions All chemical materials received from commercial sources with high purity and

used as received stock solution of lanthanum(III)1mg/mL was prepared by dissolved 0.3116g of La(NO3)3.6H2O in 9mL distilled water contain 1 mL of conc. HNO3 and dilute to 100mL with distilled in a volumetric flask , 1x10-2 M from 2- [(4-Benzyloxy phenyl)azo]- 5- Nitro-4-phenylimidazole (BANI) was prepared by dissolving 0.399 g in 100 mL chloroform by using volumetric flask. Arsenazo III, 0.05% solution is prepared by dissolving 50 mg of the reagent in 100 mL of water in volumetric flask. Format buffer pH 3.5 prepared by dissolve 60 mL of Formic acid and 28 g of NaOH in water, and dilute the solution with water to 1 liter by using of volumetric flask. Ascorbic acid solution 1% prepared by dissolve 1 g in 100mL water, in volumetric flask. [5]

Synthesis of 2- [(4- Benzyloxy phenyl)azo]- 5- nitro-4-phenyl

imidazol (BANI) This organic reagent was synthesized according to the method Shibata [6] by

dissolving (1.99 g 0.01 mole) of 4-Benzyloxyaniline in a solution of 4mL concentration HCl and 25mL distilled water After cooling this solution to 0 °C, 0.7g of Sodium nitrite dissolved in 10mL distilled water was added with maintaining the temperature at 0 °C. The mixture was left inside for 15min to complete diazotization reaction. at latter, the diazonium solution was added drop by drop to a solution of (1.89g , 0.01 mole) 5- nitro-4-phenyl imidazole and %10 Sodium hydroxide dissolved in 150mL ethanol with keeping temperature at 0 °C. After completing

34


addition , the contents were left for two hours , then added 150mL of cooled distilled water ,and the pH of the solution maintained at 6 by HCl ,brown molecules were precipitated after leaving for 24h. The solid product was filtered off, washed with cold water, crystallized twice from hot absolute ethanol and dried over CaCl2 to give yield of 80% and chemical formula of C22N5O3H17with Mw.(399.4g.mol-1).The azo reagent laboratory synthesized in this work was identified by UV – Visible, FTIR , and C.H.N elemental analysis. This reagent does not dissolve in water, but it dissolves in organic solvent such as chloroform, ethanol, acetone etc. The UV-Vis. spectrum and IR spectrum as well as the results obtained by C.H.N. study in Figures 1, 2 and Table 1 demonstrate the structure of azo ligand prepared.

Figure. 1: UV-Vis. spectrum of organic reagent 2- [(4- Benzyloxy phenyl)azo]- 5- nitro-4-phenyl

imidazol (BANI

Figure. 2: FT.IR. spectrum of organic 2- [(4- Benzyloxy phenyl)azo]- 5- nitro-4-phenyl imidazol

(BANI)

Table 1:- FTIR-spectrum of organic reagent (BANI) and Elemental analysis

Bands (cm-1) Assignments Element Theoreti

cal result Experim

ental results

3400 N-H stretching % C

65.83 65.8 3100 aromatic CH stretching

1600,1386 C=N stretching and bending % H

4.11 4.08 1450,560 –N=N- stretching and bending 1553,500 C=C stretching and bending

% N 17.45 17.41

3045 CH aliphatic 765 Ph-imidazole

35


Essential Method Take 5ml solution of organic reagent (BANI) dissolved in chloroform at 1×10-4 M

concentration shaking and adding to 5mL aqueous solution contain 80μg La(III) and shaking for 10 minutes ,afterward separate organic phase from aqueous phase and measure absorbers of organic phase at λmax of ion pair complex formed and extracted ,in addition to treated aqueous phase according to spectrophotometric method . The concentration of residual La(III) ions in aqueous phase was determined from regression line of calibration curve of La(III) in Figure 3 as well as the concentration of the extracted La(III) determined by subtraction remainder quantity from origin quantity in aqueous solution .Of stripping method for determination transferred quantity of La(III) to organic phase include shaking organic phase with three portion of 5mL 1:1 concentrated HCl and determined the stripped La(III) by Arsenazo(III) spectrophotometric method[6] the experiments show the transferred quantity of La(III) determined by Stripping equal to the same quantity determined by subtraction ,then used subtraction method to determine transferred quantity became easy and faster

Figure (3):- Calibration curve for La(III) ion in aqueous solutions by Arsenazo ( III ) spectrophotometric method

4. Results and discussion 1-Absorption UV–Vis spectrum: Absorption UV–Vis spectrum in Figure 4 shows maximum absorption for ion pair

complex extracted at λmax= 501nm

Figure 4: Absorption UV–Vis spectrum for ion pair complex

2- Effect of acidic function: Extracted 80μg La(III)in 5mL aqueous phase with 5ml of (1×10-4M) organic

reagent solution (BANI)dissolved in chloroform at different pH of aqueous phase (6-12) and shaking the two phases for (10 minutes) after that separate the two phases and determination of distribution ratio (D)as in the general method, as well as

y = 0.0049x + 0.0076 R² = 0.9981

00.10.20.30.40.50.6

0 50 100 150

Abs.

µg.La+3 /5mL

36


determine absorbance of organic phase against organic reagent as blank. The result as in figures (5,6)

Figure (5): Effect of pH on complex formation and extraction efficiency

Figure(6):D=f(pH)

The results shows optimum pH for extraction was pH=11 at the pH obtained higher absorbance and D-value that is measure reached higher extraction .Efficiency at this pH and at pH less than pH=11 suitable to reach favorable thermodynamic equilibrium for extraction and by decrease pH value increase hydrationshell of La(III)as well as increase protonated of complex agent and decrease complexation ,but at pH value more than optimum value also lead to decrease extraction efficiency.

3- Effect of Metal ion concentration: Extraction of different concentrations of La(III)ions(1-100) μg in(5mL) aqueous

solution at(pH=11) by 5mL of 1x10-4 M of (BANI) dissolved in chloroform , shaking the two layers for suitable time, and separate the two layers and determine the remainder quantity of La(III)ion in aqueous phase by followed spectrophotometric method [5], and calculation distribution ratio (D) as well as determine absorbance of organic phase at λmax=501nm against organic reagent as blank. The result was as in figures (7,8).

Figure (7): Effect of La(III) concentration

on activity of extraction and D value Figure (8): Effect of La(III) concentration

on thermodynamic equilibrium for complex formation and extraction

When we consider the concentration of metal ion in aqueous solution behaves as a factor effect on the extraction efficiency at constant other factor in solvent extraction as in equilibrium below

La(III)aq+ (BANI) org +3NO3-aq ↔ [La (BANI) ] +3;3NO-

3 org

0.1

0.15

0.2

0.25

0.3

0.35

5 7 9 11 13

Abs.

pH 1

1.05

1.1

1.15

1.2

1.25

5 7 9 11 13

Log

D

pH

-2

-1

0

1

2

0 50 100 150

LogD

µgLa(III)/5mL 0

0.050.1

0.150.2

0.250.3

0.35

0 50 100 150

Abs.

µgLa(III)/5mL

37


The results show 80µg La(III)/5mL was the optimum concentration giving higher efficiency of extraction because of the effect to increase the rate of forward direction of thermodynamic equilibrium that is mean increase formation and extraction of ion pair complex ,but any concentration of La(III) less than optimum value is not enough to reach favorable thermodynamic equilibrium that means decrease in ion association complex formation and extraction so that Absorbance and D-value .from other hand any concentration of La(III) more than optimum value effect to decline extraction efficiency and decrease absorbance[7],so D-value because effect to increase rate of backward direction of thermodynamic equilibrium according to the Lechatelier principle and mass action law. According to the theory of solvent extraction as thermodynamic method for extraction and the concentration of metal ion played in this method as thermodynamic data ,as well as the favorable state of these method depends on energy of many steps which is salvation , and hydration , partition and association controlled free energy of extraction demonstrated in the relations below:-

BANI [La(BANI)]3+;3NO-3

La3+ +3NO-3 [La(BANI)]3+;3NO3

-

organic layer

aqueous layer

The extraction depends on many steps of formation ion pair complex and partitioning between two layers and the optimum factor effect to increase formation of ion pair complex as partitioning to organic phase with more stable in this phase .

4-Effect of shaking time: For the kinetic side of the extraction methods are carried out by studying the effect

of shaking time on the extraction activity and distribution ratio values. After extracted 80μg La(III)ions in 5ml aqueous phase at (pH=11) by 5ml of (1×10-4 M) organic reagent (BANI) dissolved in chloroform by different shaking time, the results of this study in figure (9,10) demonstrate the optimum shaking time of two layers was (10min.) to reach the equilibria of extraction and at this time obtain the maximum distribution ratio value (D), and Absorbance at 501nm shaking time but less than optimum no allow to reached the equilibria of extraction, so that shaking time more than optimum favorite the dissociation equilibria and minimize the distribution ratio(D)and absorbance.

Figure (9):The relation between

distribution ratio and shaking time

Figure (10): Shaking time effect on complex

formation and extraction

0

0.2

0.4

0.6

0.8

0 5 10 15 20 25

LogD

time (min) 0

0.1

0.2

0.3

0.4

0 10 20 30

Abs.

time(min)

38


5- Effect of organic solvent: For (5mL) of aqueous solutions contain (80μg) La(III) at (pH=11) added (5mL) of

organic reagent solution dissolved in different organic solvents differ in dielectric constant (Ƹ) at (1×10-4M) . After shaking for (10min.) and separate the two layers and determine the distribution ratio (D) with each organic solvent provided the result at Table (2) which is shows there is not any linear relation between dielectric constant (Ƹ) for organic solvents and distribution ratio (D),but there is effect for organic solvent structure on distribution ratio (D). Thermodynamic parameter for extraction in different organic solvent include transfer free energy ΔGt and association constant kA as well as extraction constant kex and free energy of extraction ΔGex by application relation s below

The results in Table 2 showed free energy of transition ΔGt for La(III) ions from aqueous phase to organic phase increase with dielectric constant of organic solvents decrease but kex and ΔGex showed the high value by using Chloroform organic solvent which demonstrate sharing organic solvent and increase the stability of ion pair complex extracted and increase the approach between the cation and anion association complex extraction which is contact ion pair or loose ion pair[8]

Table(2):-Data D , ΔGex . kex , and kA for La(III) ions in different organic solvents

Organic Solvents Ƹ Dielectric constant D %E -ΔGex KAx104 Kexx108

Nitro benzene 35.740 4.900 83.120 48.54 5.19 21.26

Amyl alcohol 15.800 1.280 56.250 42.45 1.98 1.437

1,2-Dichloro ethane 10.650 5.700 85.00 49.16 5.79 27.93

Dichloro methane 9.080 1.160 53.750 41.99 1.88 1.175

Chlorobenzene 5.708 0.480 32.500 38.04 1.30 0.20

Bromo benzene 5.400 2.900 74.370 46.15 3.41 7.38

Chloroform 4.806 15.700 94.000 53.76 1.45 213.98

Benzene 2.804 3.200 76.250 46.59 3.66 8.97

Toluene 2.438 7.980 88.870 50.72 7.83 55.70

Carbone tetrachloride 2.380 8.750 89.750 51.13 8.50 66.92

6- Temperature effect: Extraction of 80 μg La(III) ion from 5mL aqueous phase at (pH = 11) by 5mL

of (1×10-4 M) (BANI) dissolved in chloroform in different temperatures at the range (5-35) after shaking the two layer for 10mintes and separate organic phase from the aqueous phase and calculate distribution ratio D at each temperature according to

39


the procedure detailled in the general method . The results as in Figures (11)and (12).

Figure:(11):D=f(TºC)

Figure (12):Kex=f(TºK)

The results show the complexation reaction and extraction thermodynamic were

exothermic behavior, and the thermodynamic data of extraction La(III) ions was illustrated in Table (3):

Table (3):- Thermodynamic data

𝑆𝑙𝑜𝑝𝑒 =−Δ𝐻𝑒𝑥2.303𝑅

ΔGex= -R T ln Kex ΔGex =ΔHex –T∆Sex

ΔHex kJ.mol-1 ΔGex kJ.mol-1 ΔSex Jk-1.mol-1 -0.067 -52.87321 190.191

The results show minimum negative value of ΔHex that reflects to approach one another ions of ion pair complex extracted by organic solution used and increase stability, as well as the approach of ion pair ions for each other may be through the formation of tight ion pair or loose ion pair and in the two cases the organic solution plays a role about increasing extraction efficiency[9].

From the other hand the negative value of Gibbs free energy ∆Gex gives us information about the spontaneously behavior in complex formation and extraction .as well as the large value of entropy ∆Sex gives very important knowledge about extraction method and telling the method of extraction was (entropic in region )[9] .

7-Synergism effect:

Extracting (80µg) La(III) in 5mL aqueous solution by 5mL of 1x10-4M organic reagent (BANI) dissolved in chloroform at (pH=11) and in presence of different concentrations of tributeylphosphate (TBP) or Methyl isobutyl ketone (MIBK) after separation of organic phase from aqueous phase ,as well as calculating distribution ratio D at each concentration of (TBP) or (MIBK),according to 8-Hydroxyquinoline spectrophotometric method [5] detailled in general method and after plotting logarithm values of distribution ratio (D) against concentration of [TBP] or [MIBK] results as in Figures (13) and (14).

0

0.5

1

1.5

2

2.5

0 10 20 30 40

log

D

T°C

slope = 3.488

8

8.5

9

9.5

10

10.5

3 3.2 3.4 3.6 3.8

log

K ex

1/TK*10-3

40


Figure(13): synergism effect with TBP

Figure(14):synergism effect with MIBK

The results show there is an enhancement in the absorbance of organic phase and in distribution ratio (D) value in presence of TBP or MIBK this result proves the organic reagent (BANI) does not saturate the coordination shell of La(III) through binding coordinatly with metal ion and then the result that suggested there is one or more molecular of water occupies in empty position ,of metal coordination shell and partitioning ion pair increases complex to the aqueous phase and dissociation and appear decline in extraction efficiency but when participating one molecular of TBP or MIBK in the coordination shell of La(III) in the complex instead of water molecule this result affect to increase hydrophobility of complex and increase partitioning to organic phase to giving rise in absorbance and D-value , as well as the slope value of straight line relation demonstrates there is one molecule of TBP or MIBK which participates in the ion pair complex extracted [La (BANI) (TBP)]3+;3NO3

- or [La (BANI) (MIBK)]3+;3NO3-.

5. Stereochemistry 1- Slope analysis method: Extraction metal La(III) from 5ml aqueous phase according to general procedure

by 5ml organic reagent solution dissolved in chloroform at different concentration(1x10-2 -1x10-6)M, sequentially separate the two layers after separate organic phase from aqueous phase, determine remain La(III) in aqueous phase and transferred quantity to organic phase and calculate distribution ratio (D) at each concentration of ligand, afterward plot log D against log[ligand] get the graph in Figure (15)

Figure(15) :- Slope analysis method

The slope of straight lines in Figure (15) demonstrates the complex extracted was 1:1 metal :ligand

2- Mole ratio method: Extraction metal La(III) from 5ml aqueous phase according to general procedure

by 5ml ligands solution dissolved in chloroform at different concentration (1x10-2 -

slope = 0.52

1

1.5

2

2.5

3

3.5

-5.5 -4.5 -3.5 -2.5 -1.5

logD

log[TBP]

slope= 0.53

0.51

1.52

2.53

3.5

-5.5 -4.5 -3.5 -2.5 -1.5

log

D

log[MIBK]

slope= 0.9

-2-101234

-7 -6 -5 -4 -3 -2

logD

log[BANI]

41


1x10-6)M sequentially separate the two layers , afterward plot absorbance vis CL/CM get the graph

Figure (16):- Mole ratio method

The graph in Figure (16) show the complex extracted was 1:1 metal : ligand, so we can suggest the following structures of the complex as shown below :

NH

N O2N

Ph

NNOC

H

H

La

3+

;NO-3

6. Spectrophotometric determination 1- Calibration curve of La(III): By applying the main procedure for extraction La(III) from 5mL aqueous

solution contain different quantities of La(III)at the range of 1-80 μg at pH=11 by 5mL of organic reagent (BANI) dissolved in chloroform at 1x10-4 M and shake for (10min). Afterward separate the organic phase from aqueous phase and measure the absorbance of organic phase at λmax=501nm against organic solution as blank and plot Absorbance against µg La(III)/5mL .And use this calibration curve for spectrophotometric determination of metal ion La(III) in different samples .

Figure(17):-Calibration curve of spectrophotometric determination of La(III)

0.007255 % RSD 1.18X10-7mol /L Detection limit 2592.89L mol-1cm-1 Ɛ 0.05357µg cm-2 Sandel’s sensitivits

2- Determination of La(III) in the selected samples Determination of La(III) ions in electronic waste equipment. as it has been clarified in the results tables (-) the study included determination of the quantities of Lanthanum ions in Laptop Screen (Toshiba ,HP) Mobile Screen (Spider, Nokia, Samsung ) and LCD Televisions (LG)and vestel. [10-11].

0.04

0.09

0.14

0.19

0.24

0.29

0.34

0.39

0 2 4 6 8 10

Abs.

CL/CM

y = 0.0037x + 0.0115 R² = 0.9959

0

0.1

0.2

0.3

0.4

0 50 100

Abs.

La3+µg

42


Table(4):- La(III) content (ppm)in waste electronic equipment

Sample type Proposed method(ppm)

RSD%

Laptop Screen Toshiba 0.570 0.75

HP 0.662 0.62

Mobile Screen Spider 0.213 0.32 Nokia 0.350 0.85

Samsung 0.721 0.14

Televisions LCD Televisions LG 1.210 0.83

Vestel 1.13 0.88

Figure(18) :- La(III) content (ppm) in waste electronic equipment

References

1.Yin, S. W., Bian, X., Luo, Y. and Zhang, F. (2013). International J. of Nonferrous Metallurgy, 2, pp: 75.

2-Sawant, V. J. and Kupwade, R. V. (2014). International Journal, 2(2), pp: 419-424.

3-Alasedi, K. M. (2009). AL-Qadisyah Journal For pure Science, 14(1), pp: 1-6.

4-Safarbali, R., Yaftian, M. R., and Zamani, A. (2016). Solvent extraction-separation of La (III), Eu (III) and Er (III) ions from aqueous chloride medium using carbamoyl-carboxylic acid extractants. Journal of Rare Earths, 34(1), pp: 91-98.

5-Marezenko, Z. and Balcerzak, M. (2000) “Separation, Preconcentration and Spectrophotometry in Inorganic Analysis”.1st ed., Elsevier Science B.V.

6-Shibata, S. M., Furukawa, M. and Nakashima, R. (1976). Journal of Analytical Chemistry, (81), p:131.

0

0.2

0.4

0.6

0.8

1

1.2

1.4

µg.g

-1

43


7-Hussein, S. A., Al-Kubaisy, R. K., & Al-Noor, T. H. (2015). Solvent Extraction Method for the Separation of Cerium (III) as Cations From Aqueous Media By use 4-[N-(5-methyl isoxazol-3-yl) benzene sulfonamide azo]-1-Naphthol Coupled With Spectroscopic Method For Determination. .Kufa Journal for Chemistry, 1(10) pp. 56-73

8-Jawad, S. K., Hameed, S. M., and Hussein, S. A. , (2011). With Solvent Extraction Method, and via new Organic Reagent 2-(Benzo thiazolyl azo)-4, 5-Diphenyl Imidazole for Spectrophotometric Determination of Copper (II) in different Samples. Iraqi National Journal of Chemistry, 43, pp299-309

9-Atkins, P. and Paula, J. de, (2010). “Physical Chemistry”. 9th ed. Great Britain:

Oxford University Press. 10-Buchert, M., Manhart, A., Bleher, D. and Pingel, D. (2012). Journal of Oeko-Institut for Applied Ecology, pp: 6-8.

11-Hurst, C. (2010). "China's Rare Earth Elements Industry". Institute for the Analysis of Global Security, Washington.

44


Characterization Of Zno /Cuo Nano Composite Preparation By Thermal Chemical Spray Pyrolysis As

Ammonia Gas Sensing

Mahdi M. Mutter1, Amel D. Hussan2 .

1 Material Researches Directorate, Ministry of Science and Technology, Baghdad, Iraq

Al-mustanceria university, collage of science, physics department2.

E-mail address: [email protected]

Abstract:

This paper reports on a chemical spray pyrolysis method to synthesize Zinc oxide thin films doping with Copper oxide at different content ranging (2,4,6) percentage,thin films used as sensor gas for Ammonia gas. The investigated and the resultant were analysis by atomic force microscopy , X-ray diffraction XRD and properties sensing. The results showed improving in structural properties where the films were polycrystalline nature with monoclinic crystal structure and uniformly distributed grains . the properties sensing also improved, where the sensitivity to ammonia gas increased with increasing the content of copper oxide.

Key words: ZnO thin films, CuO content, Spray pyrolysis, sensor gas and sensitivity.

بطریقة المحضر النحاس واوكسید الزنك اوكسید من نانوي متراكب توصیف االمونیا لغاز كمتحسس الحراري الكیمیائي الرش

2امل دشر حسین, 1د.مھدي محمود مطر

العراق, بغداد -والتكنولوجیا العلوم وزارة, المواد بحوث دائرة, مركزالفیزیاءالتطبیقیة1

الجامعة المستنصریة ,كلیة العلوم. قسم الفیزیاء 2

لخالصةا

اوكسید من بمحتوى مطعم الزنك اوكسید من رقیق غشاء لتحظیر الكیمیاوي الرش طریقة یعتمد البحث ھذا النتائج تحقیق. االمونیا لغاز كمتحسس محظر الرقیق الغشاء)% , 2,4,6( من مثبتھ مؤیة بنسب النحاس

اظھرت النتائج. التحسسیة والخواص النووي القوى ومجھر السینیة االشعة حیود باستخدام تم وتحلیلھا غیر توزع واظھرت التبلور احادیة تراكیب مع التبلور متعدد كان الغشاء ان حیث التركیبیة بالخواص تحسن

ازدیاد مع ازدادت االمونیا لغاز الحساسیة ان حیث تحسنت ایضا التحسسیة الخواص. للحبیبات متجانس .النحاس اوكسید محتوى

غازي حساس, الكیمیاوي الرش, النحاس ألوكسید محتوى, الزنك ألوكسید رقیق غشاء: المفتاحیة الكلمات .وحساسیة

45


1. Introduction

Ammonia (NH3) is generally utilized as a part of industry and the observing of its spillage has turned into an essential assignment as it is harmful (M. B. Rahmani, et al,2009). Metal-oxides (SnO2, ZnO and TiO2) based smelling salts gas sensors are being created extensively as they are more touchy to NH3 furthermore simple to manufacture (Rula M. Allaf, 2014). These sensors are, generally, of the electrical resistive-sort whose resistance differs when they are ex-postured to the recognizing gas. In any case, these sensors display upgraded gas affectability just at high working tempera-tures (above 200°C) furthermore react to numerous gasses (CO, methanol, NH3 and CH4 ) (F. Z. Haque,et al,2014). Thus, the gas affectability of metal oxide sensors are being enhanced by changing their physical properties by doping, toughening or changing their size (nonmaterial), to encourage encompassing temperature operation aeration and enhanced gas selectivity(Ganesh Kumar ,et al,2014) . In the late years, optical gas sensors in light of metal oxides as the detecting medium have been accounted for enhancing the gas sensitivity and selectivity furthermore for room temperature operation (K. Pandiadurai,et al,2013). ZnO is an imperative wurtzite-sort semiconductor with band gap vitality of 3.37 eV at room temperature and an expansive excitation restricting vitality of around 60 meV (T. Dedova,et al,2013). It likewise has fascinating compound, acoustic, optical and electrical properties. Whereas Copper (II) oxide (CuO) nanoparticles are likewise a vital inorganic semi-director with the immediate band-crevice estimation of 1.85 eV (P. Rai,et al,2012) , By which ZnO and CuO can be utilized as rising detecting materials (H. Tang, et al,2010).Several paper have been preparation of ZnO, TiO, Fe2O3, In2O3 (M. B. Rahmani, et al,2009) using different technique like vapor transport process, electrochemical deposition, chemical spray and plasma technique and other technique. Must of this technique used high temperature and high vacuum, but chemical spray requires low cast raw materials and sample preparation without vacuum for deposition(H. Tang,et al,2010).. This paper reports the results of a study on the characters-tics of a optical ammonia sensor with as-prepared and an-neared ZnO/CuO composite

2. Experimental Details

ZnO-CuO thin films were prepared by used spray chemical technique at different percentage weight of CuO which was (2, 4, 6)% percentage from weight of composite. The setup system used is showed in figure (1). The solution as pumped through the nozzle at rat flow (1 to 2) ml/minute. Gas pressure carried chemical solution was nitrogen at a pressure 4 mbar all materials produced from Merk Co. with 9870 purity.

46


Figure(1 ) Schematic of spray pyrolysis used in this work.

Table (1) slowed the parameters of chemical spray. Glass used as substrates, which it is prepared to deposed the thin film, when it was cleaned distilled water and by methan in ultrasonically for 10 minute and than part in distilled water finally dried and by smooth paper polished.

Table (1) Optimum condition of present method in this work.

The chemical solution was prepared from add CuCl in a ratios of (2, 4, 6)% percentage from 0.1M ZnCl and diluted with 100ml distill water, a accordant chemical equation down:

ZnCl2+H2O→ZnO↓ + HCl↑ ………….(1)

CuCl + H2O →CuO↓ + HCl↑ ………….(2)

Microstructure of the prepared films was confirmed by XRD type shimmed zn with CuK œ and λ=1.5406 A. thin films thickness was measured using () atomic force microscopy (AFM) was also used to studied the surface of thin filmes, which was model A2000.

47


Glass substrates were at dimension (2.5× 2.5 × 0.2)cm. The samples preparation looked by used optical microscope to sure they without detects and cracks. The sensors preparation configuration shown in figure (2). Silver past become used to restore touch wires.

Figure (2) Scheme of used sensor device.

The thickness of all samples was 400±10 nm.Thickness of films was measured after preparaed samples by Mini Test 3000 Microprocessor Coating Thickness,Germany.The system of analysis sensing show in figure (3). The voltage supply to sensor from power supply was (60) volt, and the concentration of ammonia gas was 500 ppm. The current of sensor measured by high sensitive galvanometer, current sensor indicated to electrical resistance, which it violated to the gas concentration.

Figure(3 ) diagram of sensing system used in this work.

48


3. Results an Discussion

Figure (4) shows XRD analysis of ZnO (w) ZnO: 4% CuO (b). the diffraction peaks in the diagrame agree with the valves in the (JCPDS 36-(451) for ZnO and (JCPD 5.05-00661) for CnO and we can see don’t observe other peaks in diagram, this is indicating phase purity and we obtained on crystalline ZnO. The please separation is visible confirming between ZnO and CuO. The diffraction peaks of ZnO shown in plan (100, 002, 101) and (-111, 111) for CuO, the sharp peak appears at 2Ө values at an very intense, which is around 31.31o, 33.96 o, 35.79 o for ZnO and 35.05 o, 38.29 o for CuO.

Figure( 4 ) XRD analysis (a) for ZnO and (b) for ZnO:4%CuO. Figure (5) shows the atomic force microscopy image ZnO: 4% CuO thin films at (2) and (3) dimension, 5×5µm2 sized. The surface of thin films showed well shape a film crystallites and uniform, 2D and 3D image showed the films exhibit a surface and then crystalline consequence orientation the analysis indicated the grain size are ~120nm.

Figure (5 ) AFM analysis of ZnO:4%CuO at 2 and 3 dimension.

49


Figure (6) shows the sensitivity of sensor with time to NH3 gas at room temperature. The sensitivity of sensor measured according to the equation (3 ) (G.K. Mani et al ,2013).

S%=(Ron(Ω)-Roff(Ω))/Ron(Ω)*100%........(3)

Where Ron the resistance of sensor at initial change after exposing to gas, Roff the resistance at constant after exposing to gas. A relatively short response time of sensor and recovery time after exposing to gas at 5 ppm for NH3 gas concentration. the gas sensors characterization are shown in table (2).

Table(2) The sensing characterize of ZnO:CuO gas sensors

samples response resistivity MΩ

recover resistivity MΩ

Sensitivity

As-diposited 0.675 1.10 62.967 ZnO:2%CuO 0.530 0.87 64.372 ZnO:4%CuO 0.411 0.73 77.612 znO:6%CuO 0.373 0.670 79.623

Figure (6): The resistance of sensor for all samples with time for NH3 gas.

From figure(6 ) shown the improved in the sensitivity of the thin films with increasing doping . this is mean that the resistance of ZnO decreased with increasing content CuO. However, the sensitivity approach from other spatially at content (4,6)% CuO.

4. Conclusions

In this paper the results shows that the synthesized of ZnO:CuO at deffernt percentage content of Cuocthin films at optimum conditions have good crystallites

50


and well shape and uniform in size. The sensor gas thin films deposited by spray pyrolysis. The ZnO:CuO good ability to detect NH3. From our results we observed that the sensitivity value of NH3 gas (62.962%) for ZnO as deposited, (64.37%) for ZnO:2%CuO, (77.61%) for ZnO:4%CuO and (79.62%)ZnO:6%CuO.

References

F. Z. Haque, Neha Singh, PranjalRanjan," Synthesis of ZnO/CuONanocomposite and Optical Study of Ammonia (NH3) Gas Sensing", International Journal of Scientific & Engineering Research, Volume 5, Issue 3, March-2014.

Ganesh Kumar Mani, John BoscoBalaguruRayappan," Novel and facile synthesis of randomly interconnected ZnOnanoplatelets using spray pyrolysis and their room temperature sensing characteristics", Sensors and Actuators B 198 125–133 ,2014.

G.K. Mani, J.B.B. Rayappan, A highly selective room temperature ammonia sen-sor using spray deposited zinc oxide thin film, Sens. Actuators, B 183, 459–466,2013.

H. Tang, J.C. Chang, Y. Shan, S.T. Lee, Surfactant-assisted alignment of ZnOnanocrystals to superstructures, J. Phys. Chem. B 112 (2008) 4016–4021.[36] P.D. Burton, E.J. Peterson, T.J. Boyle, A.K. Datye, Synthesis of high surface areaZnO(0001) plates as novel oxide supports for heterogeneous catalysts, Catal.Lett. 139 , 26–32,2010.

K. Pandiadurai, G.K. Mani, P. Shankar," ZnOnanospherestonanorods—morphology transition via Fe-doping", SuperlatticesMicrostruct. 62, 39–46, 2013.

M. B. Rahmani, S. H. Keshmiri , M. Shafiei , K. Latham , W. Wlodarski ," Transition from n- to p-Type of Spray Pyrolysis Deposited Cu Doped ZnO Thin Films for NO2 Sensing", SENSOR LETTERS, Vol. 7, 1–8, 2009.

P. Rai, Y.T. Yu, Citrate assisted hydrothermal synthesis of single crystalline ZnOnanoparticles for gas sensor application, Sens. Actuators, B 173 ,58–65,2012.

Rula M. Allaf and Louisa J. Hope-Weeks," Synthesis of ZnO-CuONanocomposite Aerogels by the Sol-Gel Route" Journal of Nanomaterials Volume, Article ID 491817, 9 pages2014.

T. Dedova, M. Krunks, I. OjaAcik, D. Klauson, O. Volobujeva, ," nanostructures of ZnO obtained by spray pyrolysis" , Mater. Chem. Phys. 141, 69–75. 2013.

,

51



Preparation of Some (Transition Metal-Flavylium Salt-

Substitutes Chalcon) Complexes

*Omar H. Al-Obaidi, Mohammad M. Al-Abid, Najat J. Al-Obaidi

*Chemistry department, Women Education College, Al-Anbar University Chemistry department, College of science, Al-Mustansrya University

Abstract

Three ligands were prepared and spectroscopic method and elemental

analysis verified their structures. Two of the ligands L1 and L2 are

flavylium salts and the third L3 is a chalcone. Reaction between

transition metal salts and the ligands have synthesized two groups of

new metal complexes. One group contains L1, L3 and the metal. The

other group contains L2, L3 and the metal. These complexes have been

identified by available spectroscopic tools (UV-visible ,IR and 1HNMR), the C.H.N results confirmed the proposed structures. The

experimental data disclosed that the complexes were coordinated by 6-

the coordinate with mono-and bidentate ligands forming octahedral

structure, in which L3 acts as monodentate and L1, L2 as bidentate

ligands. The metal linked with L1 and L2 through the oxygen in ortho

position in ring B, were as the linkage of the metal with L3 takes place

through the oxygen of the carbonyl group.

Keywords: Flavylium salt , metal complexes, Synthesis, Chalcone.

Introduction

In this research similar complexes prepared from different types of Flavylium salts

than that used by Takeda et al (1). And chalcone instead Flavone. These newly

prepared complexes similar to naturally occuring commelinin may have partial

applications as trace elements enriching food additives, metals carrier drugs. The

complexes may be also considered as food colorants synthesized from natural like

52



complexes, which are stable in wide pH-range. The discovery of commelinin

justified the theory of Shibata et al (2). regarding the existence that the blue color of

commelinin very stable in wide pH range and can be obtained by attacked molecular

complexes between awobanin and Flavo commelinin without the intervention of Mg

Hayashi and Takeda (3) reported at the ratio of (1:2:2) the experimental (molecular

weight) obtained for the complex agree approximately with the theoretical value to

Osawa and et al(4).

Hayashi and et al (5) extracted ablue anthocyanin (commelinin) from the petals and

found it to contain Mg. Flavone like substance and awobanin (delphinidin 3-p-6-

commaroyl glucoside-s-glucoside) Abathochromic shift have been observed in the

UV spectrum by Asem (6) when Aluminum chloride was added which indicates the

formation of Aluminum-cyanodin complexes. Many metal complexes with different

type of anthocyanins have been prepared later by other workers (7,8). The structure

of metal complexes depends upon the ratio of ligands to metal and to the Oxidation

State of the metal ion. Evidence of the structure and bonding state of the commelinin

metal was provided by ESR studies of Mg complexes, electrophoreses and IR

spectra (9-11).

Goto (12) showed that the blue color of the commelinin is very stable in wide pH

range on contrary to free anthocyanins, which is sensitive to pH variation.

In the present work commelinin like complexes have been prepared from different

transition metal using Flavylium salts and chalcone instead of Flavone.

Materials and Methods:

Experimental

Instrumentation and Chemical:

IR spectra were recorded Pye Unicam Sp. 3100 spectrophotometer, solid samples

were measured as KBr disc. For UV measurement absolute methanol and ethanol

were used as solvents. Atomic absorption spectra on Shimadzu AA-680. Rotary

evaporator RE-120 Buchi. Gallenkamp (hot stage) determined M.P. Perkin Elmer B-

240 was used for he metal analysis. BDH chemicals Ltd.-England, Fluka AG Buchs-

Swaziland and Riedel Du Haen Germany supplied chemicals.

General procedure for the Preparation of ligands:

The flavylium chloride 2-(3,4-dihydroxyphenyl)chromenylium (L1) and (L2) were

prepared as described in the literature (13).

53



3-acetoxy-2-(3,4-dihydroxyphenyl)chromenylium (L1):

Brownish red powder, m.p. 115-116 ºC, yield 84%, IR (KBr disc) shows absorption

at 3400 cm-1 (OH), 1680 cm-1 (C=O). UV-Vis shows max (EtOH) 494 nm, 274 nm.

1H NMR (100 MHz, CDCl3): 5.13 (m, 6H, Ar-H) ppm; 9.31 (s, 1H, OH),

4.3 (s, 3H, OAC); C. H. N. analysis; C=68.5 (cal. 68.4), H=4.2 (cal. 3.9).

3-chloro-2-(3,4-dihydroxyphenyl)chromenylium (L2):

orange red powder. m.p. 125-126 ºC, yield 82 %, IR (KBr disc) show adsorption at

3380 cm-1 (-OH). UV-Vis shows max (EtOH) 482 nm, 259 nm and 224 nm. 1H

NMR (100 MHz, CDCl3): 5.11 (m, 6H, Ar-H) ppm; 9.22 (s, 1H, OH), C.

H. N. analysis; C=58.18 (cal. 58.3), H=3.2 (cal. 2.6).

The substituted chalcone (L3) was prepared as described in the literature (14).

(E)-3-(3-hydroxy-4-methoxyphenyl)-1-(4-hydroxyphenyl)prop-2-en-1-oneL(3):

yellow, m.p. 79 ºC. yield 75%, IR (KBr disc) show at 1680 cm-1 C=O), 1660 (C=O).

UV-Vis show maxλ (EtOH) 323 nm, 351 nm and 328 nm , 1H NMR (100 MHz,

CDCl3): 6.35 (m, 6H, Ar-H) ppm; 9.3 (s, 1H, OH), 3.67 (ss, 1H, OCH3), C.

H. N. analysis: C=84.0 (cal. 85.2), H=5.7 (cal 5.7).

General procedure for the preparation of the complexes:

0.2 mmoles from L1 (C16H18O5) or L2 (C15H10O3) was dissolved in MeOH (30 ml)

then 0.1 mmole metal chlorides was added. The mixture refluxed for 20 min during

this time the solution became dark. A solution of L3 (C16H14O4) in methanol (0.2

mmole) was poured to the dark solution. The resulting mixture was refluxed for 30

min. and the volume of the final mixture was reduced under vacuum. The crude

products were purified by recrystallization from MeOH to give a powder, yield 82%.

The complexes are listed in Tables (1,2).

Results and discussion:

The flavylium chlorides L1 and L2 have been synthesized according to the method

devised by Robinson et al (13) through the condensation of O-hydroxy

benzaldehyde with substituted acetophenone followed by ring closure with

anhydrous hydrogen chloride. Claisen Schmidt condensation was chosen for the

synthesis of chalcone (L3). The reaction partners are acetophenone and

benzaldehyde, which condense in the presence of base in aqueous alcoholic solution

54



(14). All prepared ligands have been characterized by spectroscopic methods (UV-

Vis, IR) and C. H. N. analysis.

IR spectra:

The IR spectra exhibit the expected absorption bands of the Flavylium chlorides

(L1&L2) and chalcone (L3). In the case of the complexes, in which L3 is involved,

the carbonyl stretching frequency decreases to the range (1650-1630 cm-1), due to

the electron transfer from the ligand to the metal (9). The evidence for the linkage of

the metal to ring B in the flavylium complexes depends on the observation that an

intensive band at 1620-1610 cm-1 was observed. This band is due to the conjugation

between the C=C and C=O which occur during the chelation (9). The flavylium-

metal complexes characteristic peak at 1265 cm-1 for C-O (phenol). The -OH

stretching band at 3400 cm-1 appear broad with dimensioned intensity with, which is

indicative for complex information (15). This finding has lead us to the conclusion

that the metal was linked to ring B in each of the to flavylium ligands Table (2) .

UV-Vis spectra:

The UV-vis spectra of the complexes expected differences in the position of the

absorption bands between the ligands and the related complexes, which are due to

the coordination between the ligands and the transition metals. Appearance of new

absorption maxima is considered as a hint for the formation of complexes. The

bathochromic shift in band I upon coordination is due to the electronic transition (n

→π*) of the lone pair of electrons of the hydroxyl group in the complex Table (2).

Band III, which caused by the transition (π→π*) of the aromatic ring, exhibit

absorption maxima at 285 nm. This measured wavelength reflect the effect of

substitution by auxochromes (hydroxyl and methoxyl group). Replacement of

chloride in L1 by acetate group caused a bathochromic shift in bands I, II, and III of

the complexes (16).

Tables (2) show that the complexes of Cr, Mo, and W are deeper in color and exhibit

maxλ at considerable longer wavelength , this observation due to the occurrence of

charge transfer phenomena in trivalent metal complexes.

1H NMR Spectra: The 1H NMR spectral data of ligands (L1,L2 and L3) are

provided in the experimental part. The 1HNMR spectra of the ligands (L1 and

L2), show signals between δ 6.5-7.0 due to aromatic ring .

55



Conductivity Measurements

The measurements of the molar electrical conductivity of the complexes in methanol

are indicated in Tables (1). These results clearly show values for the molar

conductivity of the complexes of trivalent metals of group VIB namely (Cr, Mo, W)

show high values for the molar conductivity meaning that these complexes are

electrolyte (i.e. ionic).

Molar conductivity (high and low) of complexes are commonly observed depending

upon the properties of the metal and the ligands and can also be effected by the

presence of unpaired electron in the t2g eg orbitals of an octahedraly coordinated

elements.

In high spin configuration of a high ∆M value are obtained, while in case of (t2g6,

eg4) a low complexes (Cr, Mo, W) (3d3, 4d3, 5d2) (t2g eg0, t2g3 eg0, t2g2 eg0), ∆M

increased periodically due to complexation through d orbital (3d).

pH Effect Study

The complex was dissolved in methanol and buffer solution was added, a

hypsochromic shift was noticed in case of decreasing pH as shown in Fig.(1). Below

pH2 (strong acidic medium) the complexes are unstable, but a stable complex has

been observed in higher pH-values (pH=8). In contrary the anthocynin (free ligand)

is very sensitive to high pH-values. It degredates at pH above (6).

00.10.20.30.40.50.60.7

2 4 6 8 10

Abs.

pH

Fig. 1: UV-Vis. Spectra of complexes at different pH values.

The Molar – Ratio Study

The mole-ratio (4) is one of the most common spectrophotometric techniques

employed in complex studies. It is an available tool for elucidating the composition

of complex in solution. Molar-ratio (2:1) of Falvylium ligand (L1) to the metal (Cr)

56



is effected by the absorption due to change in coordinate ion of the ligand

complexes. Another molar-ratios (2:2:1, L3-L1-M) was also obtained, when chalcone

L3 was added to the above mixture as shown in Table (3) .

Fig. 2: Plot of the Cr(III) complex formation

The proposed structure : According to the results obtained from (IR, UV/visible, 1 H N M R , molar ratio, molar conductivity, atomic absorption) measurements for the prepared complexes, the proposed molecular structure of the complexes has an octahedral structure as shown in Fig.3 .

O

O

OO

O

OM

O

R R

R=OAC,Cl

HO OH

OCH3

O

OHHO

H3CO

Fig.3: The proposed structure of complexes where M= Cr(III), Mo(V) and W(VI).

00.020.040.060.08

0.10.120.140.16

0.5:1 1:01 1.5:1 2:01 2.5:1 3:01

ABS

M:L molar ratio

57



Table(1): Physical characterization ,analytical and Molar Conductance data of the compounds

Table(2): Infrared and UV-Visible Spectra data of the prepared compounds

Compound

UV-Visible

Spectra

( nm)

IR Spectra (Cm-1)

υ(C=O) υ(C-O) υ(M-O)

[Cr(L1)2(L3)2]Cl 302,444,526 1650 1210 533 m

[Mo(L1)2(L3)2]Cl3 301,423,549 1635 1220 530 w

[W(L1)2(L3)2]Cl4 306,425,522 1645 1235 535 m

[Cr(L2)2(L3)2]Cl 297,303,558 1640 1230 540 m

[Mo(L2)2(L3)2]Cl3 299,545 1625 1220 525 m

[W(L2)2(L3)2]Cl4 297,518 1630 1260 545 w

Table(3): Molar-Ratio of (L1) to (Cr) with UV-Visible Spectra data.

Molar-Ratio of

(L1) to (Cr) Max (nm) ε Mol-1 cm2 Color solution

0.5:1 562 0.034 Purple-Blue

1:1 569 0.068 =

1.5:1 565 0.094 =

2:1 563 0.120 =

2.5:1 562 0135 =

3:1 562 0.139 =

Compound Yield% Colour ΔM/Scm2 mol

-1 In DMSO

m.p οC

Metal analysis

(% found) % cal

[Cr(L1)2(L3)2]Cl 81 Purple-red 98 185-187 (4.36) 4.39

[Mo(L1)2(L3)2]Cl3 83 Purple-blue 226 170-172 (7.80) 7.82

[W(L1)2(L3)2]Cl4 85 Purple-blue 284 165-167 (13.94) 13.98

[Cr(L2)2(L3)2]Cl 80 Purple-violet 115 220-222 (4.56) 4.58

[Mo(L2)2(L3)2]Cl3 82 Purple 244 180-182 (8.12) 8.13

[W(L2)2(L3)2]Cl4 85 brown 366 183-185 (14.47) 14.50

58



Conclusion

The available experimental data suggest that the prepared L1 and L2 possesses two

coordinating sites and L3 as monodentate ligand. Physical and spectroscopic

characterization of the complexes revealed that the OH group of the flavylium and

carbonyl group of chalcone were involved in the coordination and that the Cr(III) ,

Mo(V) and W(VI) had octahedral geometry.

References

1- Hayashi K., et. al., proc. Jpn. Acad., 34, 373 (1958).

2- Shibata K., Shibata Y., and Kashiwagi, J. Am. Chm. Soc., 41, 20 (1919).

3- Takeda K., and Hayashi K. Proc. Jpn. Aca., 53, B-1 (1977).

4- Osawa Y., and et al., phytochemistry , 7, 1189 (1968).

5- Hayashi K., et al., Proc. Jpn. Acad., 34, 373 (1958).

6- Asem S., et al., phytochemistry , 11, 1139 (1972).

7- Cook, N.C.; Samman, S. Flavonoids- Chemistry, metabolism,

cardioprotective effects, and dietary sources. J. Nutr. Biochem. 1996, 2, 66–

76.

8- Teixeira S.; Siquet, C.; Aloes, C.; Boal, I.; Marques, M.P.; Borges, F.;

Lima, J.L.F.C.; Reis, S. Structure-property studies on the antioxidant

activity of flavonoids present in diet. Free Radic. Biol. Med. 2005,

39,1099–1108.

9- Malesev, D.; Kuntic, V. Investigation of metal–flavonoid chelates

and determination of flavonoids via metal– flavonoid

complexing reactions. J. Serb. Chem. Soc. 2007, 72, 921–939.

10- Ferrer, E.G.; Salinas, M.V.; Correa, M.J.; Naso, L.; Barrio, D.A..;

Etcheverry, S.B.; Lezama, L.; Rojo, T.; Williams, P.A. Synthesis,

characterization, antitumoral and osteogenic activities of

quercetin vanadyl (IV) complexes. J. Biol. Inorg. Chem. 2006, 11, 791–

801.

11- Grazul, M.; Budzisz, E.Biological activity of metal ions complexes of

chromones, coumarins and flavones. Coord. Chem. Rev. 2009, 253, 2588–

2598.

12- Go To T., et. al., Sump. Chem. Nat. Prod., 20th p.59 (1976).

59



13- Harborne J.B., et. al., “ the Flavonoids”, Chapman and Hall, London (1975).

14- Jurd L., and Horowitz R.M., J. Org. Chem., 26, 2561 (1961).

15- Pereira, R.M.S.; Andrades, N.E.D.; Paulino, N.; Bast, A.; Sawaya,

A.C.H.F.; Eberlin, M.N.; Marcucci, M.C.; Favero, G.M.; Novak, E.M.;

Bydlowski, S.P. Synthesis and characterization of metal complex

containing naringin and Cu, and its antioxidant, antimicrobial, anti

inflammatory and tumor cell Cytotoxicity. Molecules 2007, 12, 1352–

1366.

16- Lever, A.B.P. Inorganic Electronic Spectroscopy; Elsevier: Amsterdam,

The Netherlands, 1986; pp. 385–392.

60

First International Scientific Conference 29 –30 April 2017 2017نیسان 30 – 29المؤتمر العلمي الدولي األول / ISSN: Issue One /Al-Kut University College 7419 - 2414 األولكلیة الكوت الجامعة / العدد

Socio-economic Status impact on hypertension at Al- Zahra

hospital in kut city

تأثیر الحالة االجتماعیة االقتصادیة على ارتفاع ضغط الدم في مستشفى الزھراء التعلیمي في مدینة الكوت

م.م. سمیحة ناصر عبد سعید تقنیات صحة مجتمع

Sameeha Naser Abed

Master Community Health Tech. in. institute technical of kut

[email protected]

الخالصة

ارتفاع ضغط علىالخصائص االجتماعیة واالقتصادیة تأثیرتھدف الدراسة لمعرفة الھدف:

الدم.

أجریت ھذه الدراسة المقطعیة التحلیلیة في مدینة الكوت، بین تشرین الثاني :منھجیة البحث

التعلیمي , مریضا من مستشفى الزھراء 176. وتم إدخال ما مجموعھ 2017 شباطو 2016

استبیان بعد اخذ الموافقة الشفھیة وكانت المتغیرات وتمت المقابلة وجھا لوجھ باستخدام استمارة

الحالة االجتماعیة واالقتصادیة .االجتماعیة الدیموغرافیة ھي العمر والجنس واإلقامة والتعلیم

تم تحلیل البیانات باستخدام .و منخفض)على ثالث مستویات ( عال، متوسط ا: تم تصنیفھ

Minitab )16.0( .

كان و ٪62.5اإلناث ھم منارتفاع ضغط الدم ىمرض أغلب عینة الدراسة، في ھذه :النتائج

االنحراف ± ٪)، بمتوسط 82.94سنة (> 50ارتفاع ضغط الدم أكثر انتشارا في الفئة العمریة

غالبیة المرضى الذین یعانون من ارتفاع نوكا . سنة SD (59.795 ±9.276المعیاري (

مستوى بین عالقة ذات داللة إحصائیة ھناكو .ضغط الدم یقیمون في المناطق الحضریة

ارتفاع ضغط الدمو الوضع االجتماعي واالقتصادي المنخفض, التعلیم، الوضع الوظیفي

p=0.000)(

< ) سنة، ومعظم 50العمریة (غالبیة المرضى في الفئة الدراسة أن بینت : اتالستنتاجا

بین مستوى عالقة ذات داللة إحصائیةوأوضحت الدراسة وجود .المرضى ھم من اإلناث

. الدمالحالة االجتماعیة االقتصادیة وارتفاع ضغط

61



Abstract:

Objective: The objective of the study was to aimed to identify the

impact of socioeconomic status on hypertension.

Methodology: This descriptive-analytical cross sectional study was

conducted at the kut city, between November 2016 and February 2017.

A total of 176 patients were admitted in the Al Zahra hospital. Interview

was carried out by conducting a face-to-face questionnaire which

following an informed consent. The sociodemographic variables were

age , gender, residence, educational. Socio-economic status scales

(SESS): It was scored as high level, middle level and low level. The

data was analyzed using Minitab version 16.0.

Results: In this study, hypertension disease was occur in female 62.5%.

Hypertension were most prevalent in the age group 50> years (82.94%) ,

with a mean ± standard deviation (SD) of 59.795 ± 9.276 years.

Majority of hypertension patients were residence in urban. Education

level, employment status and low socioeconomic status were

significantly associated with hypertension (P-value=0.000).

Conclusion: Majority of patients occur in age group ( 50> ) years and

most of the patients are among females. There is a significant

association between SES and hypertension.

Keywords: socio-economic Status, hypertension.

1. Introduction:

Non-communicable diseases continue to be a major threats to

public health [1,2]. Worldwide , the estimated non-communicable

diseases cause 63% of deaths and it is expected to increase by 15%

between 2010 and 2020 [3[. Hypertension is among the most common

non communicable diseases [4], which is a silent killer [5]. According to

62


the national survey conducted in 2006, it is estimates that 41.50 of Iraqi

population (25- 65 years of age), have high blood pressure [6].

Interestingly, the prevalence of hypertension is still low in

the Americas at 35% , while in the African Region, the prevalence is

still higher at 46% of adults [5]. Hypertension is a contributing factor to

the development of many conditions that cause the potential risk

factors such as cardiovascular system [7], heart failure, kidney disease

[4]. Socioeconomic status (SES) has been reported to affect both

mortality and health [8] . However, socioeconomic status is significant

risk factors that commonly influenced to hypertension [9]. In fact, The

consequences of socioeconomic status on hypertension is a complex and

unclear [10]. Therefore, this study aimed to identify the impact of

socioeconomic status on hypertension.

2. Methodology:

This descriptive-analytical cross sectional study was has been

adopted to achieve the objectives of the present study. The study

conducted at the kut city, between November 2016 and February 2017.

A total of 176 patients were undertaken in the Al Zahra hospital.

Patients, whom have a known case of hypertension (previously

diagnosed by physician), were interviewed by conducting a face-to-face

questionnaire and following an informed consent. The socio-

demographic variables were age (years), gender (male, female),

residence (classified as urban or rural), educational [classified as

illiterate (who could not read and write), completed primary schooling,

secondary, institute or more] , occupation (classified as unemployed,

retired, governmental employee, private sector or housewife). Socio-

economic status scales (SESS): is one of the most important variables in

63


social science studies/researches. The scale of the 3 levels was rated on

the 3 points (Tiwari S, Kumar A scale) it was scored as high level,

middle level and low level [11]. The data was analyzed using Minitab

version 16.0 for descriptive statistics. Quantitative variables were

expressed as means ±SD while qualitative variables were expressed as

percentage and analyzed using chi-square , Fisher exact test is used

when chi-square unsuitable , The differences between observations were

considered statistical significance at a P value<0.05.

3. Results:

Table (1): This table consisted of 176 patients (66 males and 110

females) and shows that the higher percentage of patients was in the age

groups ( 50> ) years (82.94%) . With a mean ± standard deviation (SD) of

59.795 ± 9.276 years.

Table (1 ) Distribution of patients according to age and gender

Figure (1) Shows that male 37.5% of patients and female 62.5% of patients.

Age (years) Males Females Total

No. % No. % No. %

50≤ 10 15.15 20 18.18 30 17.05

50> 56 84.85 90 81.82 146 82.95

Total 66 100 110 100 176 100

Mean±SD (Range) 59.795 ± 9.276

64


Figure (4.1) The Distribution of patients according to gender.

Concerning education level, the higher percentage of males were

secondary education level 36.36 %, while the lower percentage 18.18%

was illiterate, and the higher percentage of females 66.36% was in

illiterate, while the lower percentage 3.64% was in institute & higher

education level, with a statistically significant (P-value=0.00).

In respect to employment status, the higher percentage of males

45.45% were retired and 87.27% of females were housewives. However,

statistical significance have been proved for this point (P-value=0.000).

As shown in this table, 100% of males and 98.87% of females

were residing in an urban area, with not statistically significant (P-

value=0.5286). (Table 2)

Female 62.5%

Male 37.5%

Gender

65


Table (2): The Distribution of patients is according to Demographic variables.

Demographic variables

Male Female Total

P-value No. % No. % No. %

Education level

Illiterate 12 18.18 73 66.36 85 48.29

0.000* HS

Primary 14 21.21 17 15.45 31 17.61

Secondary 24 36.36 16 14.55 40 22.72

Institute &Higher 16 24.24 4 3.64 20 11.36

Total 66 100 110 100 176 100

Employment status

Unemployed 18 27.27 2 1.82 20 11.36

0.000**

HS

Retired 30 45.45 6 5.45 36 20.45

Government employed 10 15.15 6 5.45 16 9.09

Private 8 12.12 0 0 8 4.54

Housewife 0 0 96 87.27 96 54.54

Total 66 100 110 100 176 100

Residence

Urban 66 100 108 98.18 174 98.87 0.

5286***

NS

Rural 0 0 2 1.82 2 1.139

Total 66 100 110 100 176 100

*p-value calculated after inducing primary, secondary and institute &higher education into one. **p-value calculated after inducing retired, Unemployed and housewives into one and inducing government employ, private into one. *** Fisher exact test

Table (3) was edited to verify the distribution of the patients

according to socioeconomic Status. It was shown that the higher

percentage of the males (63.64%) were in moderate scale of socio

economic status(SES) and for females (80.91%) were in low SES,

66


while lower percentage of males (24.24%) and females (80.91%)

were in high scale SES. There was a significant association between

SES and hypertension (P-value =0.000) Table (3) Distribution of patients according to socioeconomic Status.

Socio-Economic

Status

Male Female Total P-value

No. % No. % No. %

High (>80) 8 12.12 2 1.82 10 5.7

*0.000 HS

Moderate (60--80) 42 63.64 19 17.27 61 34.65

Low (<60) 16 24.24 89 80.91 105 59.65

Total 66 100 110 100 176 100

*p-value calculated after inducing High, Moderate into one.

4. Discussion:

Some studies have shown male and female to be associated with

hypertension and the strong association in female as compare with

male[12]. In this study, females had the higher percentage 62.5% of

hypertension which agrees with other studies that were done by

Bonaventure Amandi, 2012 in South Africa [13], N Folb et al, 2016 in

South Africa [9], and Hakan Tüzün et al, 2015 in Turkey [3]. They

found that females comprise 71.9%, 75% and 61.2% of the patients

respectively. Regarding the age, the results of this study demonstrated

that 82.94% of patients were in age group >50 years. These findings

were similar to those obtained from study done by N Folb et al, 2016 in

South Africa [9], who found that half of patients were in age group of >

50 years. It is evident that hypertension is a disease of old age. In this

study, the mean age of patients was 59.795 ± 9.276 years. These results

were nearly similar to the study of David Conen et al, 2009 in USA

67


[14], who found that the mean age of patients was 54+7 years.

Education, occupation and residence are significant risk factors that

commonly associated with hypertension [10]. In this study, the higher

percentage of patients 48.29% was alliterated. The association between

hypertension and education was statistically significant (p-value=0.000).

Which disagrees with Bonaventure Amandi, 2012 in South Africa [13] ,

who found that most of the study samples 59.1% were in secondary

school , while Girma Fikadu et al, 2016 in Ethiopia [4], who found that

the association was statistically not significant. Although the

association between hypertension and occupation was statistically

significant (p-value=0.000), hypertension occurs more among

unemployed and housewife 65.9 %, which similar to Bonaventure

Amandi, 2012 in South Africa [13], who reported that the highest

percentage of patients were among unemployed 75.9%. (33.3%). This

conclusion may be explained according to data from the WFP survey

(2004), it is shown that about 80% of adult males in Iraq were

employed as compare with 13% of females[15] . On other hand, this

finding was opposite to the study of Girma Fikadu et al , 2016 in

Ethiopia [4], who found no significant association between hypertension

and occupation . In concerning to the residence, 98.87% of cases in this

study were living in urban area, which disagrees with the study that was

done by Bonaventure Amandi, 2012 in South Africa [13], who found

that most of the hypertension patients 50.38 % were among rural area. A

much higher prevalence of hypertension in high income countries was

found previously [16]. Many studies has been stated the association

between lower socioeconomic status (SES) and hypertension [17]. In

this study, the highest frequency of patients (59.65%) was of low SES

while the 5.7% were of high SES. The association between hypertension

68


and SES were significantly (p-value=0.000). Sintayehu Asfaw, 2012 in

Norway [12], reported independently association between hypertension

and SES. Similarly, in the U.S, hypertension is more prevalent lower

SES class as compare with higher SES class [18]. This might be related

to Iraq's economic and social changes due to wars, more than one

decade of sanctions and inappropriate policies [15].

4. Conclusions:

Majority of patients occur in age group ( 50> ) years and most of

the patients are among females. There is a significant association

between education level and employment status with hypertension but

the association with residence were not significant. There is a

significant association between SES and hypertension.

Recommendations:

Health education of community about hypertension, complication,

potential risk factors, proper use of therapy and an important of periodic

examination of patients. Improving socioeconomic and Modifying

lifestyle through acquiring healthy habits such as increasing physical

activity, smoking cessation and avoiding as much as possible stress and

anxiety, in addition to a healthy diet provided by health care

professionals and by implementing a proper system of social education,

as well as promoting more effective health services.

References:

1. Jiaojiao Wang, Jian James Ma, Jiaqi Liu1, Daniel Dajun Zeng1,

Cynthia Song, Zhidong Cao (2017). Prevalence and Risk Factors of

Comorbidities among Hypertensive Patients in China. International

Journal of Medical Sciences; 14(3): 201-212.

69


2. Juliana Kagura,Linda S Adair, Pedro T Pisa, Paula L Griffiths, John

M Pettifor, Shane A Norris(2016). Association of socioeconomic

status change between infancy and adolescence, and blood pressure,

in South African young adults: Birth to Twenty Cohort. BMJ

Open;6.

3. Hakan Tüzün, Sefer Aycan, Mustafa Necmi İlhan (2015). Impact of

comorbidity and socioeconomic status on quality of life in patients

with chronic disease who attend primary health care centres. Cent

Eur J Public Health; 23 (3): 188–194.

4. Girma Fikadu and Seblewengel Lemma (2016). Socioeconomic

Status and Hypertension among Teachers and Bankers in Addis

Ababa, Ethiopia. International Journal of Hypertension.

5. World Health Organization (2013). A global brief on Hypertension

,Silent killer, global public health crisis.

6. Ministry of Health, Ministry of Planning and Amman, WHO (2007).

National Survey for Non-Communicable Diseases Risk Factors in

Iraq.

7. Carline Francois (2015). Hypertension Knowledge, Medication

Adherence, and Self-efficacy Skills Among African American

Males in New York City, (M.Sc.) Monroe College.

8. Aino Lammintausta (2013). Effects of Socioeconomic Status and

sociodemographic features on cardiovascular disease mortality and

morbidity in Finland, (PhD) University of Turku.

9. N Folb , M O Bachmann, E D Bateman, K Steyn, N S Levitt V

Timmerman, C Lombard, T A Gaziano, L R Fairall (2016).

Socioeconomic and modifiable predictors of blood pressure control

for hypertension in primary care attenders in the Western Cape,

South Africa . Afr Med J;106(12):1241-1246.

70


10. Grotto, Itamar, Huerta, Michael Sharabi, Yehonatan (2008).

Hypertension and socioeconomic status. Cardiology ,23 (4).

11. Tiwari S, Kumar A. (2005). Development of standardization of a

scale to measure socio-economic status in urban and rural

communities in India. Indian. J. Med; 122: 309-314.

12. Sintayehu Asfaw (2012). Contribution of Risk Factors to

Socioeconomic Variation in Blood Pressure: the Tromsø study,

(M.Sc.) University of Tromsø.

13. Bonaventure Amandi Egbujie (2012). Relationship between

Socioeconomic status and cardiovascular disease in black South

Africans living in a rural and an urban community, (M.Sc.)

University of the Western Cape.

14. David Conen, Robert J. Glynn, Paul M Ridker, Julie E. Buring, and

Michelle A. Albert (2009). Socioeconomic status, blood pressure

progression, and incident hypertension in a prospective cohort of

female health professionals. European Heart Journal ; 30, 1378–

1384.

15. Ala'din Alwan (2004). Health in Iraq, Ministry of Health, Second

Edition.

16. Annibale Cois, and Rodney Ehrlich (2014). Analysing the

socioeconomic determinants of hypertension in South Africa: a

structural equation modelling approach . BMC Public Health;

14:414.

17. Colin Bell, Linda S. Adair, Barry M. Popkin (2004). Understanding

the role of mediating risk factors and proxy effects in the association

between socio economic status and untreated hypertension. Social

Science & Medicine 59: 275–283.

71


18. E. Miranda Reiter (2014). The Impact of Social Support,

Psychosocial Characteristics, and Contextual Factors on Racial

Disparities in Hypertension , (PhD) Utah State University.

72

First International Scientific Conference 29 –30 April 2017 2017نیسان 30 – 29المؤتمر العلمي الدولي األول / ISSN: Issue One /Al-Kut University College 7419 - 2414 األولالجامعة / العدد كلیة الكوت

Study of electrical characteristics of PS/Si heterojunction

prepared by photo-electrochemical etching

Ayad Zwayen Mohammed

-Laser & Optoelectronics Engineering Department- University of Technology

Abstract :

in this work, N-type Silicon was etched using 650 nm laser

wavelength and 20 m W power density with using beam expander.

Different etching times were applied on five single crystalline bulk

Silicon wafer to obtain hetero junction devise. Electrical properties by

means of forward and reverse biased dark current and capacitance –

voltage were investigated in order to examine how well the device is

performed .

keywords : photo electrochemical etching, hetero junction, dark current

الخالصة :

طول موجي يباستخدام لیزر ذ n حفر سلیكون من نوع ,في ھذا العمل

استخدم ملي واط وباستخدام موسع حزمة , 20نانومتر وبكثافة قدرة مقدارھا 650

زمن حفر مختلف لتحضیر خمس عینات من شریحة سلیكون احادي التبلور, وذلك

لكي یتم الحصول على مفرق ھجین . الخصائص الكھربائیة كتیار الظالم في حالة

التحفیز االمامي والعكسي و متسعة جھد تم دراستھا لكي یتم التعرف عى مدى

جودة اداء الجھاز .

1-introduction

Porous silicon is a very promising material due to its excellent

optical, thermal and photoelectrical properties, its obvious compatibility

with silicon-based microelectronics and its low cost[1], Its large surface

73


area within a small volume, its controllable pore sizes, its convenient

surface chemistry, and the ability to modulate its refractive index as a

function of depth makes porous silicon a suitable dielectric material for

the formation of multilayers [2] .The formation of fine network with

very small voids (often called pores) surrounded by thin walls (often

called Nano crystallites) made it demonstrated efficient, tunable, room

temperature light emission at energies above the used band gap related

IR luminescence of bulk Si [3,4]. Thus one can make used of such

property in fabrication of efficient optoelectronic devices by increasing

light trapping in the active region, due to its morphology which could be

manipulate it by changing different etching conditions such as etching

time, solution concentration power density of laser ect.[5,6]

2-Experimental work

the substrate used in this experiment is n-type silicon wafer with

orientation of 100. Wafers were cleaned to remove any oxide layer

formed on the Si substrate etched with cleaning solution consisting of

(HNO3, CH 3COOH, HF) at ratios (2:1:1:10) [7], to remove oxides by

placing wafers in the ultrasonic machine (Cerry PUL 125 device) for 15

minutes, then cleaning them by alcohol and ultrasonic machine for 15

minutes, then cleaned by water and ultrasonic waves for additional 15

minutes.

P Si layers were fabricated using photo electrochemical method,

by dipping Si wafer in (40%) concentration HF solution, then

illuminating it with diode laser of (650) nm wavelength and (20) m W

power density at different etching time of (5, 10, 15, 20, 25) min. Figure

(1) shows the scheme for photo electro chemical (PEC) method [8]

74


Figure (1 ) Scheme for PEC method

Electrical properties of the formed heterojunction were measured

for forward and reverse current under dark condition and capacitance –

voltage characteristics.

3-Results an discussion

The electrical behavior of P-Si/C-Si structure under dark

condition and in reverse and forward biasing is illustrated in figure (2).

Results of five samples prepared at different etching times (5, 10, 15,

20, 25 min) show a good diode behavior.Increasing etching time means

it was getting small nano size and different electrical characteristics at

each current density obtained [9],when increasing etching the long

etching time increases the current resistance of porous silicon. Our

results agrees with other worker results, thus we may conclude that the

current density decreases with increasing the etching time , which has

different ideality factors and saturation region in J-V [9].

75


Figure (2) I-V characteristices of P-Si sample at different etching times.

Figure( 3) shows the capacitance at reverse biasing for samples prepared

at different etching times. Results show increase in capacitance for

samples with increasing etching time from 5min to 25 min,This increase

may be due to photo electrochemical etching process developed the

depletion layer are the charge carriers depleted from the substrate

silicon. The capacitance of the samples was found to increase with the

specific surface area. However, the capacitance per unit sample area

showed a decreasing trend with the specific area, and this has been

attributed to the increase in resistance that would probably result from

the deepening of the pores upon etching [10].

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Figure (3) Capacitance voltage characteristics for Psi at different etching

time.

The built in potentials of the prepared samples agree with the

capacitance value at different etching times, this result is shown in

figure(4). The reverse bias voltage was ranged through (0.1-1.2) V, the

cross point (1/C2=0) of the (1/C2-V) curve represents the built-in

potential of the heterojunction [11].

Figure (4) The built in optional value of etched silicon at different etching time.

77


Conclusion

From this work we could conclude that effect of time etching has a great

influence on electrical properties of porous silicon . The change in the

electrical properties may be due to the great change in surface

morphology my mean of change in porosity layer and the size of pore

and the wall between them .

Reference

1. N. Naderi, M.R. Hashim, " Effect of Surface Morphology on

Electrical Properties of Electrochemically-Etched Porous Silicon

Photodetectors",Int.J.Electrochem.Sci,Vol.7,pp. 1512– 1518,2012.

2. Elisabet Xifré Pérez,” design, fabrication and characterization of

porous silicon multilayer optical devices", Universitat Rovira I

Virgili, chapter 2, pp. 5, 2007.

3. L. T. Canham, " Silicon quantum wire array fabrication by

electrochemical and chemical dissolution of wafers", Appl. Phys.

Lett., Vol. 57, pp. 1046, 1990.

4. Evan T Salem "Carrier life time, Time constant and other elated

Detector Parameter for Porous Silicon /Silicon Heterojunction

detector", Eng. & Tech. Journal, Vol. 28, No. 18, pp. 5660, 2010.

5. Khaldun A. Salman, Khalid Omar, Z. Hassan, "The effect of

etching time of porous silicon on solar cell performance" ,Vol. 50

,pp. 647–658, 2011.

6. Uday Muhsin Nayef, "Fabrication and characteristics of porous

silicon for photo conversion", International Journal of Basic &

Applied Sciences, Vol.13 No.02.

7. Shinji Yae," Structural change in Porous Si by Photo illumination

during metal particle enhanced etching", Research Department of

78


Materials Science and Chemistry, Graduate School of

Engineering, University of Hyogo.

8. Alwan M.alwan and Narges Z.Abd al Zahra,” The influence of

heating treatment on physical properties of porous silicon" journal

of al-Nahrain University, vol.12 (2), pp.76-81, 2009.

9. Ahmed K. Al-Kadumi, Alwan M. Alwan, Ali H. Al-Batat, ,"The

effect of the etching time on the electrical properties of nano

structure silicon", Iraqi Journal of Physics, Vol.10, No.18, pp.1-4,

2012.

10. To.Chi Weng and Hsisheng Teng,” Characterization of High

Porosity Carbon Electrodes Derived from Mesophase Pitch for

Electric Double-Layer Capacitors”, Journal of The

Electrochemical Society Vol.148, issue 4, pp. A368-A373, 2001 .

11. H. H. Afify, S. H. EL-Hefnawi, A. Y. Eliwa" Realization and

Characterization of ZnO/n-Si Solar Cells by Spray Pyrolysis",

Egypt. J. Solids, Vol. 28, No. 2, pp .243-254, 2005.

79


Effect Of Continuous Wave Laser Diode Light–Curing On The Thermal Expansion Of Nano-Composite Resin

Thoalfiqar Ali Zaher, Muna Youhana Slewa, Hanaa Nafee.Azeez

College of Education, Dept. of Physics, University of Al Hamdaniya.

Abstract

Several important properties associated with continues wave diode laser polymerization lights and dental materials treated using diode laser technology, such as temperature rise, material thickness and cure time have been reviewed in this paper. During the polymerization of resin composite specimens of Ivoclar Vivadent Tetric N-Ceram Light Cured Hybrid restorative composite resin were prepared. Temperature rise was measured using a type L digital thermocouple, the temperature measurements were performed at depths(1,2,3)mm from the top of the composite for all specimens . The Composite was irradiated using direct(Power=86.3 mW) and reflected(Power=33.6 mW) light from diode laser (wavelength=405 nm). For each exposure time three specimens were prepared. We observed the maximum temperature rise of(5ºC) for direct laser light and (0.8ºC) for reflected light. Temperatures rise did not reach the critical value that can cause pulpal ,enamel and dentine damage by virtue of a prominent safety feature of laser diode radiation , which ensures that no excessive heat is produced by two curing modes.

الملخصدراسة العدید من الخصائص المهمة المرتبطة ضوء لیزر دایود ذو الموجة المستمرة عند في هذا البحث تم

مه في بلمرة مواد طب األسنان ومعاملتها استخدام هذه التكنولوجیا مثل ارتفاع درجة الحرارة، سمك استخداخالل استخدمت عینات من المواد المستخدمة في قسم العالج التحفظي لطب االسنان المادة وزمن المعالجة .

. ارتفاع درجة Ivoclar Vivadent Tetric N-Ceram Light Cured Hybrid وتسمى البلمرة . تم قیاس درجة الحرارة للمادة المربة لكل العینات L نوع رقمي حراري مزدوجاستخدام هقیاس تمالحرارة

ملي 86.3(طاقة عوملت بنمطین من اشعة لیزر الدایود االول شعاع مباشر المادة. ملم)1,2,3عند اسماك(لوحظ اعلى ارتفاع في .وتم تحضیر ثالثة تماذج لكل زمن تعرض ملي واط) 33.6(طاقة واالخر منعكس واط)

) عند استخدام نمط م0.8º) عند استخدام الضوء الباشر للیزر و(م5ºدرجة حرارة المادة تحت االختبار وانت (او ،العاج لب السن صل إلى القیمة الحرجة التي مكن أن تسبب تلف الحرارة لم اتدرجارتفاع الضوء المنعكس

خالل حالتي ، والتي تضمن عدم إنتاج الحرارة المفرطة الدایود لیزرحكم میزة السالمة البارزة إلشعاع المینا .العالج اللیزر

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Introduction

The increasing rate of production of light activated dental materials

has made curing units essential and common devices of each dental

office. They are used to polymerize light activated composite

resins[1].Decreased curing time for dental treatment is an important

aspect of clinical success. Recently, the diode laser has been marketed

as an alternative to conventional light-curing units for quick, safe, and

effective polymerizing of composite resins[2].

the photo initiator in most visible light– cured adhesives, is highly

sensitive to light in the blue region of the visible light spectrum and has

a peak area of absorption at 470 nm.[3–5]. Wavelengths outside this

blue band have little or no effect in stimulating to initiate the

polymerization reaction[3,4,5].

The light output characteristics of commonly used visible-light-curing

units have been found to be inconsistent[4,6]. These units produce light

that has a broad (120 nm) bandwidth that typically falls between 400

nm and 520 nm[3,4,5].The resultant energy density is commonly

around 400 mW/cm2, with the light intensity decaying at geometric

progression with distance[2,5,6].In contrast, laser light has a single,

narrow band of wavelength that travels in parallel waves that are in

phase spatially and temporally[2,7].

Attempts have been made to increase the output energy of

conventional curing lights, but adding intensity without narrowing the

bandwidth may be hazardous to the tooth due to heat buildup[2] .With

diode laser, the power output and curing time may be consequential

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determinants of its thermal effect upon the pulp[8].However, Powell et

al. have determined that at energy densities needed for laser

polymerization of light-cured materials, no apparent damage would be

expected to the pulp, dentine and enamel. Recent studies are

inconclusive regarding the ideal laser curing time; in vitro tests have

been performed with limited sample sizes and without thermal

cycling[8,9].

The detrimental effect of temperature increase on pulp tissue during

restorative treatment has been of concern to clinicians. External

application of heat to a tooth can cause pulpal trauma if the magnitude

and duration of the temperature increase reaches a critical level

[10,11,12].

Dental treatments often result in an increase of temperature at the

tooth surface and ultimately in the dental pulp. An increase of the

intra pulpal temperature (exceeding 11.5°C) can result in irreversible

damage to the pulp tissue[13].

NANOCERAM-BRIGHT is a light cure Nano-hybrid composite

composed of a special blend of micro and Nano fillers which produces

a superior restorative. The highest aesthetic results have been achieved

through the development of a sophisticated method for the integration

of the nanoparticles in the resin matrix. These nanoparticles of average

particle size of 20nm, assist in a quick polish after placement as well as

ultralow wear. It is characterized by ease in sculpting with no

slumping. Its low polymerization shrinkage due to high loading and

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particle size blending yields high marginal integrity, minimizing post-

operative sensitivity and eliminating micro leakage[14].

The free radical polymerization is given in three steps: Initiator (I),

Propagation (p) and Termination (t). These three steps have individual

rates of polymerization, The monomer grows to polymers under the

free radical chain reaction of polymerization. The photochemistry

explains the interaction between the light and matter to induce

chemical reaction. The dental adhesive chemical reaction is induced

with the curing light, which is an electromagnetic spectrum of a

wavelength range of the ultraviolet and visible light. Two molecules in

special arrangement select this kind of initiation of polymerization[

3,15].The absorption of the electromagnetic energy is given in the

equation (1) :

hv=hc/λ (1)

Initiation. I = hc / λ (2)

λ= Wavelength of the incident light curing, ~ 550 nm in the dental adhesive.

h= Planck’s constant

c= Velocity of light.

The electromagnetic initiator energy is absorbed and temporarily

stored as excited electron, moving at very high-speed along the chain,

initiating the photo polymerization with the energy given by equation

(2). The photo polymerization initiation absorbs the light, induces the

free radical or ion and is proportional to the monomer concentration.

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The light does not affect the chain of propagation and termination. An

important advantage in the dental adhesive field is that the initiation

starts at a large range of temperature[16].

The addition of photosensitizers to the monomers induces the

absorption of light with specific wavelength, disassociating the free

radical, giving energy to the monomers for the propagation and

termination process. The propagation speed is based on the (s) bond in

the new bonding restoration, from the less stable p-Bond of the hybrid

layer, composite filling, and residual tooth[2,3,16 ].

The aim of this study was to compare the thermal effect of direct and

reflect light of continues wave laser diode on different depths, thermal

expansion properties of dental Nano composites material.

Material and method

This section describe the experimental system to realize the aim of this

research, the design and construction of our experimental apparatus,

which formed a major part of present research works .The whole

experiment setup was designed and constructed in our lab .This

allowed us effective control over the system parameter. The composite

tested in this study was Ivoclar Vivadent Tetric N-Ceram Light Cured

Hybrid restorative composite resin Fig.(1,b). The samples were cured

by applying the diode laser beam at wavelength of 405 nm, the output

of the diode laser beam was measured before the polymerization using

light detector. The BNC output signal is the direct photo current out

of the photodiode anode and is a function of the incident light power

(p) and wavelength (λ) can be obtained from the spectral responsivity

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curve included in datasheets for DET10A .We converted the

photocurrent to a voltage (vout) for viewing on digital voltmeter . This

is accomplished by adding an external load resistance Rload output

power is found as:

Pout = Vout / R (A) × Rload (3)

All other specification can be found in data sheet of the DET10A ,then

power of the diode laser beam was checked and recorded . For direct

laser beam was equal to (86.3 mW) and for reflect laser beam was

equal to (33.68 mW). Cylindrical specimens of each composite were

prepared with plastic molds of 10 mm of length and a diameter of 8

mm and compressed at (1,2,3 mm) thickness then polymerized for two

minutes .The cured composite material high was measured in three

different places with Digital Caliper ,its accurate equal(±0.02)mm and

the mean value was registered as the depth of cure. Fig.(1) shows the

heatsink compound, Nano-hybird composite digital thermocouple,

cylindrical plastic, and digital thermocouple used in this research

work.

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The beam emerging from the diode laser was first incident to an

object . The object beam was collimated on the upper surface of the

sample, the video camera was mounted over the specimen .The timer

was used of each measurement to determine the final time of the photo

polymerization, beam-splitter was positioned at an angle in the path of

the diode laser such that a portion of the incident beam was reflected

and then incident to an object .Fig. (2) illustrate the test set up which

consisted of a diode laser, beam splitter , nanoparticle material ,

thermocouple, video camera and timer .

(b) Nano-hybrid composite

(a) Heatsink compounds

(d) Digital thermocouple ( c ) Plastic cylindrical

Fig. (1) the instruments and material of the experiment

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Fig.( 2) The schematics and figures of the direct and reflect experimental apparatus

Resin composite specimens were polymerized from above to prevent

direct warming for probe temperature by the light source diode laser.

The accuracy of L digital thermocouple is ( ± 0.1°C), WE added Heat

sink compounds material to improve the probe temperature reading

.The temperature for Nano Ceram and time of laser radiation were

recorded simultaneously using digital video camera GALAXY NOT 5

and the time resolution of this measurements was determined by

frame of camera system which is about 1/60, then the measurements

analyzed with help of a personal computer .

Reflect

Direct

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Results and Discussion

Fig.3 show the temperature increase with exposure time when curing the dental materials at different thickness (1,2,3)mm for direct diode laser radiation. At (1,2,3 mm) thickness an increase in irradiate time from (1 – 70 ) sec produced significant increase in temperature . Above this reading of time , the temperature was almost constant.

Change temperatures of composite resins during (1 – 120 )sec of exposure time for direct radiation and variable in thickness of material at ( 1 mm) temperature increase(ΔT) was (5 ᵒ C) ,at (2mm) thickness the temperature increase(ΔT) was(4.5 ᵒ C)and at (3mm) thickness the temperature increase(ΔT) was (3.7 ᵒ C) were shown in Tab.1.

Fig.3The relation between temperature increase with exposure time when curing the dental materials at different thickness (1,2,3)mm for direct diode laser radiation.

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Table 1. Change temperatures of composite resins and variable in thickness of

material in mm during (1 – 120 )sec of exposure time for direct radiation

Material thickness

(mm)

Temperature increase

ΔT (ᵒ C)

1 5

2 4.5

3 3.7

Fig.4 show the temperature increase with exposure time when curing

the dental materials at different thickness (1,2,3)mm for reflected laser

light radiation.

Fig.4 The relation between temperature increase with exposure time when curing the dental materials at different thickness (1,2,3)mm for reflect diode laser radiation

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An increase in irradiate time from (1 – 100 ) sec produced an

increase in temperature of material about (0.8ᵒ C) , (0.4ᵒ C) and (0.1ᵒ

C) at thicknesses (1,2,3) mm respectively , above this reading of time ,

the temperature was almost remain constant. Table 2. shows the

change of temperature of composite resins at variable thickness of

material in mm during (1 – 120 )sec of exposure time for reflect laser

light radiation.

Table 2. Change temperatures of composite resins and variable in thickness of

material in mm during (1 – 180 )sec of exposure time for reflect radiation

Material thickness

(mm)

Temperature increase

ΔT (ᵒ C)

1 0.8

2 0,4

3 0.1

As light passes through the mass of the resin composite its intensity is

greatly decreased due to light absorption and scattering by restorative

material attenuating its potential to cure . This is inconsistency with

the significant and gradual reduction in temperature observed when

the depth of the composite material increased . Thus the resin

composites evaluated shouldn’t be cured in 2 mm or less especially for

divert light of diode laser[2,16 ].Both direct and reflected light from

laser diode light . curing sufficiently polymerized composite to a depth

of 2 mm which is the value acceptable for clinical application[18 ].

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Thickness of cure is considered as an essential physical property of

composite resin and is widely used to evaluate the polymerization

efficiency of light activated composite. The use of diode laser for

composite resin curing has increased because it produces a low

increase in temperature during its use. They have a narrow spectral

range which matches the optimum absorption wavelength for the

activation of the camphor Quinone[17].

Conclusions

Diode laser beam was used to measure the thermal expansion of Nano

composites resin. The investigation showed that the temperature

values were significantly influenced by the interaction among resin,

exposure time and depth. Both direct and reflected light of laser diode

sufficiently polymerized composite to a depth of 2mm which is the

value acceptable for clinical application.

References

1- Boaro LC, Gonçalves F, Guimarães TC, Ferracane JL, Versluis A, Braga RR. (Polymerization stress, shrinkage and elastic modulus of current low-shrinkage restorative composites Dent Mater)2010 Dec;26 (12): 1144-50.

2- Cipolla AJ. (Laser Curing of Photoactivated Restorative Materials) 1993 Salt Lake City, Utah: ILT Systems; 1–3.

3- van Noort R. (Introduction to dental materials) Edinburgh, 2009 4- Netto AM, Steinhaus J, Hausnerova B, Moeginger B and Blümich B.

(Time-Resolved Study of the Photo-Curing Process of Dental Resins with the NMR-MOUSE Appl Magn Reson) 2013; 44:1027–1039.

5- Wikipedia (2011) http://en.wikipedia.org/wiki/

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6- Rohlin, A., (What is tungsten copper use for) (2011) www.ehow.com

7- Bhatia, R.(Materials Issues and Engineering Design Considerations for Device Packaging of High Power Edge Emitting Semiconductor Laser Arrays and Monolithic Stacked Laser Diode Bars)(2003)”, Department of Chemical & Materials Engineering, San Jose State University, California.

8- Stansbury JW.(Curing Dental Resins and Composites by Photopolymerization) J Esthet Restor Dent, 2000; 12:300–308.

9- Stansbury JW.( Dimethacrylate network formation and polymer property evolution as determined by the selection of monomers and curing conditions) Dent Mater, 2012; 28:13–22.

10- Kurchak M, Desantos B, Powers J, Turner D. Argon laser for light-curing adhesives. J Clin Orthod. 1997;31:371–374. Sedivy M, Ferguson D, Dhuru V, Kittleson R. Orthodontic resin adhesive cured with argon laser: tensile bond strength [abstract 582]. J Dent Res. 1993;72:176.

11- Schneider LFJ, Consani S, Sinhoreti MAC, Sobrinho LC, Milan FM. Temperature change and hardness with different resin composites and photo-activation methods. Oper Dent 2005; 30: 516-521.

12- Powell GL, Morton TH, Whisenant BK. Argon laser oral safety parameters for teeth. Lasers Surg Med. 1993;13:548–552.

13- Bing-Hong Shih (On the optical properties and microstructures of GaN films inserted with low-temperature Al0.8Ga0.2N interlayers )2005 Journal of Crystal Growth 276 362.

14- https://www.net32.com/ec/nanoceram-bright-shade-bl2-bleach-white-syringe-d-121445.

15- Uhl A, Mills RW, Jandt KD. (Polymerization and light-induced heat of dental composites cured with LED and halogen technology) Biomater. 2003; 24:1809–1820.

16- Uhl A, Völpel A, Sigusch BW.(Influence of heat from light curing units and dental composite polymerization on cells in vitro) J Dent. 2006 Apr;34(4):298-306.

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https://www.net32.com/ec/nanoceram-bright-shade-bl2-bleach-white-syringe-d-121445

https://www.net32.com/ec/nanoceram-bright-shade-bl2-bleach-white-syringe-d-121445


17- Tsaia PC, Meyers IA, Walsh LJ. Depth of cure and surface micro hardness of composite resin cured with blue LED curing lights. Dent Mater 2004; 20:3649.

18- Watts DC, Amer O, Combe EC. Characteristics of visible-light activated composite systems. Br Dent J 1984; 156:209-15.

19- Schattenberg A, Lichtenberg D, Stender E, Willershausen B,Ernst CP. Minimal exposure time of different LED-curingdevices. Dent Mater 2008; 24:1043-9. Epub 2008 Jan.

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A feasibility study of PV - battery- fuel cell hybrid energy system for rural electricity supply in Iraq

Mohammed Ridha Saeed Alhendawi1, Ali Saleh Aziz2 Al-Hussain University College, Karbala, Iraq.

[email protected], [email protected]

Abstract: Nowadays, the conventional fossil energy resources such as coal, petroleum, and natural gas, which meet most of energy demand in the word, are being rapidly exhausted. Also, their consumption causes environmental problems such as the greenhouse effect and pollution of the air and water. Therefore, renewable energy sources are attracting more interest as an alternative source of energy. Iraq enjoys a massive amount of solar radiation throughout the year so that Photovoltaic (PV) system could be a suitable choice to supply electricity as an off-grid energy system. The aim of this research paper is to design an optimal standalone PV/battery/fuel cell hybrid energy system for a remote off-grid village in Iraq. HOMER software is used as a tool for the feasibility study of the proposed system. The simulation results show that the optimum hybrid power system consists of 86 kW PV, 30 units of battery, and 10 kW fuel cell is justified on technical and economic grounds for the future. In addition, the comparison between the proposed system, PV/battery, and PV/fuel cell has been done. The results indicates that PV/battery is the cheapest energy system, while PV/fuel cell is technically feasible, but still not economically viable.

) الھیدروجین وقود خالیا - بطاریات - شمسیة الواح( الھجین الطاقھ نظام جدوى دراسةالعراق في نائیة منطقة لكھربة

2، علي صالح عزیز 1الھنداوي رضا سعید محمد

.كلیة الحسین الجامعة، كربالء، العراق

في الوقت الحاضر، یتم استنفاد موارد الطاقة األحفوریة التقلیدیة مثل الفحم : الخالصةوالبترول والغاز الطبیعي التي تلبي معظم الطلب على الطاقة بسرعة فائقة . باالضافة الى ان

من المشاكل البیئیة مثل ظاھرة االحتباس الحراري وتلوث الھواء استھالكھا یسبب الكثیر یتمتع والماء. لذلك، تجذب مصادر الطاقة المتجددة المزید من االھتمام كمصدر بدیل للطاقة.

العراق بكمیة ھائلة من اإلشعاع الشمسي على مدار العام بحیث یكون استخدام االلواح الكھربائیة . یھدف ھذا البحث الى تصمیم نظام طاقة الشمسیة خیارا مناسبا لتوفیر الطاقة

متكون من االلواح الشمسیة وبطاریات و خالیا وقود الھیدروجین لقریة نائیة معزولة كھربائیة عن الشبكة الوطنیة. برنامج ھومر سیتم استخدامھ كوسیلة لدراسة جدوى النظام المقترح.

30كیلو واط من االلواح الشمسیة و 86ون من اظھرت النتائج ان نظام الطاقة الھجین المتك

94



كیلو واط من خالیا وقود الھیدروجین ھو النظام االمثل من 10وحده من البطاریات مع

الناحیة التقنیة واالقتصادیة للمستقبل. باالضافة الى ذلك تم اجراء مقارنة بین النظام المستخدم ظام االلواح الشمسیھ مع خالیا وقود مع كل من نظام االلواح الشمسیة مع البطاریات ون

الھیدروجین. تبین من خالل النتائج ان نظام االلواح الشمسیة مع البطاریات ھو ارخص نظام بینما یعتبر نظام االلواح الشمسیة مع خالیا وقود الھیدروجین مجدي من الناحیة الفنیة ولكن

الیزال نظام غیر اقتصادي.

Keywords: Hybrid, Solar radiation, Fuel Cell, HOMER software, Total net present cost (NPC)

1. Introduction

Nowadays, the landscape of the energy is characterized by the continual growing in global demand, depleting of fossil fuels, climate change, and rising prices [1].

One of the main worldwide issues is to minimize the emissions of conventional power plants and to reduce the high cost of feeding electricity for remote regions [2].

In 2012, during the declaration as the “International Year for Sustainable Energy for All” (SE4ALL), the International Renewable Energy Agency (IRENA) established a roadmap in order to double the participation of renewable energy in the universal energy mix from the existing 20% to around 40% by 2030. The goal of that is to switch power generation sector of developing countries for exploiting and absorbing further renewable energy sources, upgrading and modernizing outdated grid systems, providing new and innovative solutions [3].

Despite the availability of fossil fuels in Iraq, energy shortages problems initiated in 1991 because of the distractions caused by the overall ruin of the country. Furthermore, many rural villages in Iraq are located far away from the grid. Solar energy can play a great role in the growing of energy of the area through minimizing the using of conventional fossil fuels. The country enjoys an enormous amount of solar radiation in the most days of the year [4]. Since solar energy has an intermittent nature, storing of energy is needed. Lead acid batteries are commonly utilized for this purpose. High energy efficiency and comparatively low price are some features of these batteries. On the other hand, they have many limitations such as high cost of maintenance, complication, low capacity during winter season, high carbon footprint, large size, and costly to dispose of after utilize. Therefore, novel hybrid energy systems are tested in order to

95


minimize the required number of batteries as much as possible. However, the batteries are important, since they relieve transient processes in hybrid energy systems using renewable energy sources and fuel cells [5].

In order to find the optimal design of hybrid energy systems for the rural regions, several studies have been done. In reference [4] the authors used HOMER software for optimization to investigate the best economic hybrid energy system for remote area in Iraq. They found that off-grid hybrid PV/diesel system is a suitable choice for the selected site.

The authors in reference [6]; addressed the simulation and optimization approaches to the use of hybrid energy systems in two modes, standalone and grid-connected. They showed that the replacement of diesel generators with hydrogen systems is not economically applicable. It is essential to reduce the cost of hydrogen technologies in the future to make the system cost within acceptable range.

In this research paper the simulation of hybrid energy system consists of Solar Photovoltaic together with Fuel Cell, and battery storage has been performed and a power management strategy has been designed to find the optimum feasible system. The results of the proposed system are compared with PV/battery and PV/Fuel Cell energy systems in terms of techniques and economics.

2. Materials and Methods

2.1. HOMER Software

HOMER is a software used to implement techno- economic analysis on a hybrid generation energy systems. An hourly simulation of each feasible combination of components is performed. Moreover, HOMER simulation can perform “sensitivity analysis” in which the amounts of some parameters are varied to investigate their impact on the cost of energy [7].

2.2. Description of the Selected Village

For this study, the chosen standalone remote rural village is Budjah, a small hamlet in Muqdadiyah district, Diyala, Iraq. This area is not connected to the grid, which offers an opportunity for standalone electrification of the village.

2.2.1. Load Profile

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The selected residential unit is simple and requires few amount of electrical energy consumed for lighting and electrical appliances. The daily load profile of the village is shown in figure 1 [8]. In order to assessment the variances which may be taken place daily, a random variability of 20% is applied for both day-to- day and time-step-to-time-step.

Figure 1: Daily load profile of the village

2.2.2. Solar Radiation Resource

Iraq is one the countries characterized by remarkable potency in solar radiation. The area is blessed with about 340 sunny days a year. The data of solar radiation is taken for Muqdadiyah village at a location of 33°58' N latitude and 44°56' E longitude [8]. Figure 2 shows the monthly average daily radiation of the selected village. It is clear that during the summer season, highest level of solar radiation is recorded with a daily radiation of 7.56 kWh/m2/d in June. It attains its lowest level in the winter season with a daily radiation of 2.6 kWh/m2/d in December. Influence of ambient temperature on the power of the PV array are considered in this study. The average monthly air temperature of the selected village is shown in figure 3.

Figure 2: Solar energy profile at the selected village

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Figure 3: Monthly ambient temperature of the selected village

2.3. System Components 2.3.1 System Description and Details of the Components (PV) modules, battery, electrolyzer, hydrogen tank, fuel cell, and inverter are the main components of the system. For each of these equipment, the cost, number of units to be used, operating hours, etc. need to be specified in HOMER software. The production of electricity from the renewable device will be supplied into AC load. Description of these components is explained in this section. Tables 1, 2, 3, 4, 5, and 6 present the input parameters and costs of PV, fuel cell, electrolyzer, hydrogen tank, battery, and inverter respectively. The costs of the components have been taken from different references [3, 9, 10, and 11].

Table 1. PV inputs details

Parameter Value De-rating factor 90 %

Nominal operating cell temperature 47 °C Temperature coefficient -0.5% / °C

Efficiency at standard test condition 13 % Ground reflectance 20%

Capital cost $ 4000/kW Replacement cost $ 2500/kW

Operating and maintenance cost $ 10 /kW/year Lifetime 25 years

Tracking system No Tracking

Table 2: Fuel cell inputs details

Parameter Value Type DC


Operating and maintenance cost $ 0.02/kW/hr Lifetime 5 years

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Table 3: Electrolyzer inputs details

Parameter Value Type DC

Efficiency 75% Capital cost $ 2000/kW

Replacement cost $ 1500/kW Operating and maintenance cost $ 20 /kW/year

Lifetime 15 years

Table 4: hydrogen tank inputs details Parameter Value



Table 5: Battery inputs details Parameters Value

Nominal voltage 2V Nominal capacity 1500 Ah (3 kWh)

Cost of capital $ 508 Cost of replacement $ 475

Cost of operating and maintenance $18 /yr Minimum lifetime 5 years

Table 6: Inverter inputs details Parameter Value Efficiency 90%



2.3.2. Operating Principle The principle of operation is to use the photovoltaic system to directly supply the load whenever possible to reduce the fuel cell and battery losses. When excess PV energy is available, power is supplied first to the batteries, then to an electrolyzer, which turns on for producing hydrogen, which is delivered to the hydrogen storage tanks. The batteries or the fuel cell is then utilized to feed the load when the PV

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output is insufficient to feed the load. Based on the total cost of the devices, HOMER decides whether to supply energy from the fuel cell, battery, or both. The schematic diagram of this system is shown in figure 4. The configuration of the proposed system in HOMER software is presented in figure 5.

Figure 4: Schematic diagram of the proposed system

Figure 5: The configuration of the proposed system in HOMER

software

2.4. Cost Optimization Firstly, the technical feasibility of the capability of the system to feed the load demand is accessed by HOMER. In the next step, it determines

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the net present cost (total cost of the project) which comprise capital cost, replacement costs, operation and maintenance costs, fuel costs and salvage by using [12]:

NPC = CtotCRF(i.n)

(1) where Ctot is the total cost per year ($/year), i is the real interest rate (%) per year and n is the lifetime of the project. The capital recovery factor (CRF) is calculated using [12]: CRF(i. n) = i×(1+i)n

(1+i)n−1 (2)

The amount of net present cost is determined by taking into account the salvage cost (SC) which is the residual value of the system components at the end of the project lifetime and is calculated using 12]: SC = CRC × Trem

Tcom (3)

Here CRC is the cost of replacement ($), Trem is the remaining life (year) and Tcom is the lifetime (year) of the component. The levelized cost of energy (COE) yields [12]: COE = Ctot

Etot (4)

Where Etot is the annual consumption of the total electricity (kWh/year).

3. Simulations and Results

3.1. Optimization Results

Simulation has been executed based on projection period of 25 years with an interest rate of 6%. The system operation is simulated in HOMER by considering the hourly data and determining the balance of energy for each of the 8760 hours per year. For each of the 24 hours in the day, it makes a comparison between the capacity of the system for supplying the energy and the energy demand by determining the feasibility of the system and estimating the lifecycle cost. After simulating the system, 756 feasible solutions are found and out of these, 23 bestead feasible systems classified according to net present cost (NPC) are shown in figure 6. It presents that the best optimum result is achieved when the system is composed of 86 kW of PV arrays, 10 kW fuel cell turbine, 30 units of batteries, 30 kW sized inverter, 54 kW electrolyzer, and 15 kg hydrogen tank. The simulation result also shows that the second optimum system is for 85 kW of PV arrays, 10 kW fuel cell turbine, 30 units of batteries, 30 kW sized inverter, 55 kW electrolyzer, and 16 kg hydrogen tank. The second feasible system is more expensive than the first one since the total cost of supplying

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electricity from hydrogen system is higher than PV total cost. It is essential to be mentioned that there are no fuel cost and emissions for the all feasible systems since they do not include generators in their components.

Figure 6: The overall optimization results showing system configuration sorted by total net present cost

3.2. Economic Analysis

Figure 7 shows the cash flow summary of the net present cost. It is clear that PV cost contributes the highest cost to the overall cost. It is because of the capital cost of PV module is high. Furthermore, it can be noticed that the cost of electrolyzer is the second highest capital cost. It is essential to be highlighted that the electrolyzer should be replaced by a new one since the life time of the electrolyzer is only 15 years. Therefore, the replacement cost of electrolyzer considerably increase the total cost of the system. Batteries, fuel cell, hydrogen tank, and inverter also contribute to the total cost but with less ratio. The best optimal energy system was found to have an initial cost of $ 540740, annual operating cost of $ 9042/year, replacement cost of $ 74184, salvage cost of $-8810, total net present cost (NPC) of $ 656,333, and levelized cost of energy (COE) of $0.986/kWh.

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Figure 7: Cash flow summary of PV/fuel cell/battery energy system

Simulation is done for both PV/battery and PV/fuel cell in order to make economic comparison between these systems and the propose PV/fuel cell/battery system. The results show that the PV/battery system (48 kW PV, 150 units of batteries, and 30 kW converter) has a total NPC of $ 358958 which is 45% cheaper than the PV/fuel cell/battery system. On the other hand, PV/fuel cell system (102 kW PV, 25 kW fuel cell, 30 kW converter, 73 kW electrolyzer, and 36 kg hydrogen tank) system is found to have a total NPC of $ 887800 which is 35% more expensive than the proposed system. Figure 8 presents the cash flow summary of PV/battery energy system while the cash flow summary of PV/fuel cell energy system is shown in figure 9.

Figure 8: Cash flow summary of PV/battery energy system

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Figure 9: Cash flow summary of PV/fuel cell energy system

3.3. Energy Production Analysis Figure 10 shows the production of energy for 19th of January. It is clear that PV module begins to generate power at 06:30 AM until 06:30 PM. This energy is used to supply the load with the desired power output. However, during 04:30 PM to 05:30 PM, the PV power and batteries is not enough to feed the load, so, fuel cell works to compensate for the lack of power during these periods. During the night hours, the output of PV become zero, therefore, the fuel cell and batteries will supply the load. Furthermore, battery state of charge reaches its maximum value at 04:30 PM and minimum value at the sunlight hours (06:30 AM to 04:30 PM). Table 7 presents summary of important electrical output results. It indicates that PV and batteries penetration is 85%, the fuel cell penetration only 15% of the total energy production. Furthermore, the excess electricity is found to be 17.8 % which can be exploited to supply deferrable load. Some of the activities performed by the deferrable load are water pumping and ice making.

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Figure 10: Mix of energy production by the proposed system

Table 7: Summary of important electrical output results

Production KWh/yr Percentage (%) PV array 147074 15 Fuel Cell 26235 85

Total 173309 100 Consumption KWh/yr Percentage (%)

AC primary load 52069 39 Electrolyzer load 82796 61

Total 134864 100 Quantity KWh/yr Percentage (%)

Excess electricity 30881 17.8 Capacity shortage 563 1.1

4. Conclusion The optimal design of a photovoltaic/battery/fuel cell hybrid energy system to supply the electric load demand of a remote rural village in Iraq is discussed in this research paper. The proposed optimal design study focuses on techno-economic performance. The simulation results show that a hybrid energy system (86 kW PV arrays, 10 kW fuel cell turbine, 30 units of batteries, 30 kW sized inverter, 54 kW electrolyzer, and 15 kg hydrogen tank) is the optimal feasible solution for the village. The results are compared with the PV/battery and PV/fuel cell hybrid energy system. Although the proposed system is more expensive than PV/battery system, however, there are many concerns associated with the handling of batteries. Inserting hydrogen storage technology can reduce the required number of batteries. PV/fuel cell system is not economically viable since it has very high net present cost. Taken into

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account that the price of hydrogen storage system is expected to fall, therefore, PV/battery/fuel cell hybrid energy system can be technically and economically viable in the future.

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