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1 MİLLİ GELİRDEN ÖNEMLİ BİR KAYBIMIZ! KOROZYON DERGİSİ Derginin amacı, korozyonu önlemenin bilimsel ve teknolojik altyapısına ilişkin gelişmelerin izlendiği ve bunların özümlenmesi ve uygulamaya aktarılması imkân ve mekanizmalarının tartışılarak değerlendirildiği bir forum olarak etkili olabilmektir. Korozyon Dergisi nde konu ile ilgili olmak üzere Türkçe ve İngilizce de özgün makaleler, çeviri yazıları, öncelikle uygulama alanına hitap eden araştırma sonuçları, uygulama alanında edinilen bilgi ve deneyimlerin konu alındığı yazılar, tarama ve tanıma yazıları, konferans raporları ve kitap eleştirileri yayınlanır. Korozyon Dergisi ne gönderilecek yazılar 14 daktilo sayfasını geçmeyecek şekilde aşağıdaki düzende hazırlanmalıdır: (1) Makale başlığı (Türkçe ve İngilizce), (2) Yazar(lar)ın ad(lar)ı, (3) Yazar(lar)ın 50 kelimeyi geçmeyen kısa özgeçmiş(ler)i, (4) 100 kelimeyi geçmeyen Türkçe ve İngilizce özetler, (5) Makale, (6) Kaynakça. Yazarların makale yazım kuralları olarak Korozyon Dergisi nde daha önce yayınlanmış yazıları örnek almaları önerilir. JOURNAL OF CORROSION The objective of the journal is to provide an effective forum for the investigation of developments related to the scientific and technological infrastructure of corrosion prevention, as also for the discussion and evalution of adaption and application possibilities and procedures for these developments. The journal publishes original articles, translations, research results, especially related to practical applications, papers treating information from case-studies, survey and review articles, conference reports and book reviews in English and Turkish on the subject or corrosion. Contributions to the journal should not excead 14 typed pages in length and be prepared in the manner given below: (1) Title of article (Turkish and English) (2) Name(s) of author(s) (3) Biographical data of author(s) not exceed 50 words (4) Turkish and English summaries not to exceed 100 words each (5) Text of the article and (6) References. Authors may consult articles published in back issues of the journal for guidance in the preparation of their manuscripts. SAHİBİ / OWNER KOROZYON DERNEĞİ THE CORROSION ASSOCIATION YAYIN YÖNETMENİ PUBLISHING DIRECTOR Mustafa Doruk Orta Doğu Teknik Üniversitesi, Ankara YAYIN KURULU PUBLISHING BOARD Mustafa Doruk Orta Doğu Teknik Üniversitesi, Ankara Saadet Üneri Ankara Üniversitesi, Ankara Ali Fuat Çakır İstanbul Teknik Üniversitesi, İstanbul Semra Bilgiç Ankara Üniversitesi, Ankara Necil Kurtkaya Elek. Y. Muh. Oktay Akat AKAT Mühendislik A.Ş. Ankara YAYIN DANIŞMA KURULU PUBLISHING ADVISORY BOARD Hayri Yalçın Gazi Üniversitesi, Ankara Mehmet Erbil Çukurova Üniversitesi, Adana Ahmet Çakır Dokuz Eylül Üniversitesi, İzmir Mustafa Ürgen İstanbul Teknik Üniversitesi, İstanbul Melike Kabasakaloğlu Gazi Üniversitesi, Ankara Gözen Bereket Osmangazi Üniversitesi, Eskişehir Timur Koç Gazi Üniversitesi, Ankara Kadri Aydınol Orta Doğu Teknik Üniversitesi, Ankara Fatma Erdem Türkiye Şeker Fab. A.Ş., Ankara Vedat Yalçın Noksel Çelik Boru Sanayi A.Ş. Yves M. Günaltun Petroleum Institute of Abu Dhabi Abu Dhabi Kemal Nişancıoğlu Norwegian Institute of Technology NTH-Trondheim, Norway M.Tettamanti De Nora S.p.A., Milano, İtaly H.M. Shalaby Kuwait Institute for Scientific Research, Kuwait KOROZYON DERGİSİ yılda iki defa olmak üzere Korozyon Derneği tarafından yayınlanır ve ücretsiz olarak dağıtılır. Yazışma adresi : Korozyon Derneği, Orta Doğu Teknik Üniversitesi, Metalurji ve Malzeme Mühendisliği Bölümü, ANKARA JOURNAL OF CORROSION is published two times a year by the Corrosion Association in Turkey, Department of Metalurgical and Materials Engineering, Middle East Technical University, ANKARA/TURKEY Tel : (90-312) Tele-Fax : (90-312) , Dizgi ve Baskı : Poyraz Ofset - ANKARA Tel : (312) Fax : (312)

2 DAHA İYİ KOROZYON KONTROLÜ İLE DAHA GÜVENLİ BİR DÜNYA EUROCORR 2012 YE YAKLAŞIRKEN! Korozyon Derneği nin bu yıl ev sahipliğini üslendiği Avrupa Korozyon Kongresi (EUROCORR) ne kısa bir süre kaldı. Bilindiği gibi, bu etkinlik Korozyon Derneği nin de üyesi olduğu Avrupa Korozyon Federasyonu (EFC) tarafından her yıl üye ülkelerden birinde düzenlenmektedir. Bu yıl, 9-13 Eylül 2012 tarihlerinde İstanbul da, Sheraton Maslak Otelde yapılacak bu uluslar arası etkinliğe 700 den fazla bilim insanının katılması beklenmektedir. EFC Yöneticiler Kurulu son olağan toplantısını 27 Mart 2012 günü İstanbul da yaptı. Kurulun rutin gündemi kapsamında EUROCORR 2012 ye sunulan bildiri özetleri de değerlendirildi. Toplam 702 bildiri önerisinden 432 adedi sözlü, geri kalan 270 adedi de poster sunulu bildiri olarak kabul edildi. EUROCORR 2012 ye ülkemizin üniversiteleri, araştırma kurumları ve sanayi kesiminden sunulan bildiri sayısı beklentilerimizi aşarak 83 rakamına ulaştı. Bunlardan 27 si sözlü geri kalanları ise poster sunulu bildiri olarak kabul gördü. Bildiri özetlerinin ülkelere göre dağılımından öne çıkan önemli olgulardan biri çevremizdeki komşu ülkelerden ulaşan yoğun katılma isteğidir. Açıktır ki, EUROCORR 2012 Türkiye ve çevresindeki Orta Doğu ve Kafkasya ülkelerinde mevcut bilimsel çalışmalar ve araştırma potansiyelinin uluslar arası ortamda tanıtımı için eşsiz bir fırsat sunacaktır. EUROCORR 2012 fevkalade yoğun programı yanında öğrenciler, akademisyenler ve uygulayıcılara yönelik bir dizi etkinliklere de yer verecek. Bunlardan biri akademik ve sanayi ortamlarında görevli araştırmacılar için öngörülen, öğrencilerin de katılabileceği ileri seviye kursudur. İstanbul Teknik Üniversitesi Maslak Kampusunda 7-9 Eylül 2012 günlerinde gerçekleştirecek bu etkinlik İsveç Kraliyet Teknoloji Enstitüsü (KTH) den Prof. Christofer Leygraf tarafından yönetilecek. EUROCORR 2012 çatısı altında yer alacak diğer etkinliklere de kısaca değinelim: Sürtünmeli Korozyon (Tribocorrosion) Bilimi ve Teknolojisi Kursu: 11 Eylül 2012 Salı günü verilecek bu kursla öğrenciler, genç araştırmacılar, makine ve kimya mühendisleri, biyo mühendisler, malzeme uzmanları ve bakım personeline sürtünmeli korozyonun mekanizması ve önlenmesinde başvurulabilecek yaklaşımlar tanıtılacak. Prof. Jean-Pierre Celis (KU Leuven, Bel- SAFER WORLD WITH BETTER CORROSION CONTROL AS WE APPROACH TO EUROCORR 2012! Not much left to the European Corrosion Congress (EUROCORR), to be hosted by Corrosion Association this year. As known, this activity is held every year in one of its member countries by European Corrosion Federation (EFC), to which Corrosion Association is a member. This year more than 700 scientists are expected to participate in this international activity to be held at Sheraton Maslak Hotel in Istanbul, between September 9-13, EFC Board of Directors held its last meeting in Istanbul on March 27, Abstracts of papers to be presented in EUROCORR 2012 were also considered within the routine agenda of the Board. Out of 702 paper proposals in total, 432 were accepted as oral presentations and the remaining 270 were accepted as poster presentations. Number of papers submitted to EUROCORR 2012 from our universities, research institutes, and industrial organizations reached to 83, which exceeded our expectations. Out of this figure 27 were accepted as oral presentations and the remaining were accepted as poster presentations. One of the prominent facts in the submitted paper abstracts based on their distribution to countries is the intense participation desire received from neighboring countries. It is clear that EUROCORR 2012 will be an unequaled opportunity for Turkey and surrounding Middle Eastern and Caucasian countries to introduce their existing scientific studies and research potential. Besides the extremely dense program of EURO- CORR 2012, there will be a series of activities for students, academics, and practitioners. Among these is the advanced course, which is considered for researches working in academic and industrial mediums, as well as students. To be held at Maslak Campus of Istanbul Technical University on September 7-9, 2012, this activity will be moderated by Prof. Christofer Leygraf from Swedish Royal Technology Institute (KTH). Let us remember briefly other activities to be held under EUROCORR 2012: Tribocorrosion Science and Technology Course: Mechanism of tribocorrosion and approaches to prevent it shall be introduced to students, budding researchers, mechanical and chemical engineers, bioengineers, material specialists, and maintenance personnel in this course to be held on Tuesday, September 11, Led by Prof. Jean-Pierre Celis (KU Leuven, Belgium)

3 çika) ve Prof. Pierre Ponthiaux ( Ecole Centrale, Paris/Fransa) yönetilecek bu kurs dokuz derslik bir seriden oluşacak. Havacılık Çalıştayı : EUROCORR kapsamında ilk defa bu yıl düzenlenecek olan bu etkinlik 11 Eylül 2012 Salı günü gerçekleştirilecek. Önde gelen havacılık şirketleri ve araştırma kurumlarından katılacak uzmanlar havacılık sektörünün gereksindiği korozyonu önleme yaklaşımlarını tartışarak değerlendirecekler. Öncelikle kapsanacak konular (a) çevreden kaynaklanan korozyonun kontrolünde geleneksel yaklaşımlar (kromatlar ve kadmiyum) yerini alabilecek seçenek yöntemler, (b) Yeni kuşak korozyon kontrol sistemlerini oluşturacak temel öğeler, (c) Korozyonunun modellenmesi, yavaşlatma ve öz- koruma kavramlarında gelişmeler, ve (d) korozyonun teşhisi, analizi ve korozif ortamlara ilişkin değerlendirmeler üzerinde yoğunlaşacak. Ortam Destekli Çatlamaların (ODÇ) Oluşumu ve Mekanizmaları Çalıştayı: EFC çatısı altında faaliyet gösteren çalışma gruplarının katkıları ile düzenlenecek bu çalıştay 10 Eylül 2012 Pazartesi günü yapılacak. Çalıştayın birincil amacı akademisyen ve uygulayıcıları buluşturarak ODÇ nin mekanizmaları, teşhisi ve yorumlanmasında ulaşılan seviye ve yetersizlikler hakkında görüş alışverişinin yapılabileceği bir platform oluşturmaktır. Bu çalıştayda öne çıkacak konular (a) ODÇ oluşumlarının kapsam ve türleri, ve (b) ODÇ nin mekanizması ve modellenmesi olarak özetlenebilir. Gelişmekte Olan Ülkeler İçin Su Çalıştayı: EFC ve Dünya Korozyon Organizasyonu (WCO) nun ortak katkıları ile düzenlenecek bu çalıştay 12 Eylül 2012 Çarşamba günü yapılacaktır. Gelişmekte olan ülkelerin yaklaşık altıda birinde güvenli su kaynaklarına ulaşılamadığı ve içme suyunda oluşan korozyonun ciddi sağlık sorunlarına neden olabildiği gerçeğinden hareketle suyun iletimi, depolanması ve dağıtımında izlenecek etkili yaklaşımlar bu çalıştayda tartışılarak değerlendirilecek. EUROCORR 2012 ile ilgili diğer ayrıntılara EFC nin web sayfasından (http://www.efcweb.org) veya adresinden ulaşabilirsiniz EUROCORR 2012 İLE GELEN MUTLULUK Avrupa Korozyon Federasyonu tarafından korozyon bilimi ve mühendisliği alanında seçkin katkıları ile öne çıkan genç bilim adamlarına verilen Kurt and Prof. Pierre Ponthiaux (Ecole Centrale, Paris/France), this course shall consist of a series of nine classes. Aviation Workshop: This activity, which will be held for the first time under EUROCORR this year, shall be held on Tuesday, September 11, Experts participating from leading aviation companies and research institutions shall discuss and evaluate the methods to prevent corrosion required in the aviation sector. The main topics to be discussed shall focus on (a) options and methods to substitute traditional approaches (chromates and cadmium) in control of corrosion caused by the environment, (b) fundamental elements to constitute the new generation corrosion control systems, (c) improvements in corrosion modeling, slowdown and self-protection concepts, and (d) diagnostics, analysis of corrosion and evaluations regarding corrosive mediums. Workshop only Occurrence and Mechanisms of Environmentally Assisted Fracture (EAF): This workshop organized with the contributions of workgroups working under EFC shall be held on Monday, September 10, The primary purpose of the workshop is to create a platform where academics meet with practitioners to exchange views on the level reached and inadequacies regarding EAF mechanisms, diagnosis, and interpretation. The topics to be highlighted in this workshop may be summarized as (a) Scope and types of EAF formation and (b) mechanism and modeling of EAF. Workshop on Water for Developing Countries: This workshop shall be held jointly by EFC and WCO (World Corrosion Organization) Wednesday, September 12, Effective approaches on transmission, storage and distribution of water shall be held in this workshop, based on the fact that in approximately one out of six developing countries safe water sources cannot be reached and corrosion in drinking water creates serious health problems. For more detailed information on EOROCORR 2012 please visit EFC website (http://www.efcweb. org) or website. BLISS WITH EUROCORR 2012 This year Assoc. Prof. Ramazan Solmaz, faculty member in Department of Chemistry in Faculty of Science-Literature of Bitlis University and a full member of Corrosion Association, was awarded

4 ları ile öne çıkan genç bilim adamlarına verilen Kurt Schwabe ödülünün bu yılki kazananı Bitlis Üniversitesi, Fen-Edebiyat Fakültesi Kimya Bölümü öğretim üyesi ve Korozyon Derneği nin asil üyelerinden Doç.Dr.Ramazan Solmaz! Ülkemiz korozyon topluluğu için onur kaynağı olan bu önemli başarısı nedeni ile Doç.Dr.Ramazan Solmaz ı Korozyon Derneği adına içten kutluyoruz. Ödül verilme gerekçesini EFC-2012 Nisan ayı E- bülteninden aktararak dergimizin bu sayısında okurlarımızın bilgisine sunuyoruz. Ayrıca Dr. Solmaz ın özgeçmişi, fotografı ve 2008 yılında Electrochemica Acta dergisinde yayımlanan ve en çok atıf alan yayın ödülüne değer görülen Investigation of adsorption and inhibitive effect of 2-mercaptothiazoline on corrosion of mild steel in hydrochloric acid media başlıklı makalesini de Dergimizin bu sayısında bulabilirsiniz. BETONARME YAPILARI TEHDİT EDEN TEHLİKE: KOROZYON 6 Nisan 2012 günü sel sularına direnemeyip yıkılan ve 15 vatandaşımızın ölümü ile sonuçlanan Çaycuma Filyos Çayı üzerinde kurulu betonarme köprü faciası ve son dönemlerde sıklaşarak ülkemizin neredeyse tamamını kuşatan depremler en ileri düzeyde alarm veriyor! Açıktır ki, betonarme yapıların tasarımı ve inşaatında korozyon olgusunu göz ardı etmenin ulusumuza yükleyeceği bedel giderek ağırlaşacaktır. Korozyon Derneği olarak üniversitelerimizi, araştırma kurumlarımızı, sivil toplum örgütlerimizi ve devletimizin ilgili kurumlarını göreve çağırıyoruz! Betonarme yapıların tasarımı ve yapımında görev alacak teknik personelin bilgi altyapısındaki bu boşluk en kısa sürede giderilmelidir. Bu çağrımız öncelikle Üniversitelerimiz ve ilgili bölümlerine yöneliktir. Mühendislik ve mimarlık eğitimi veren bölümlerimizin programlarını korozyon dersleri ve korozyon araştırmaları ile güçlendirmelerini öneriyor ve bekliyoruz. Kuruluş amaçları ve üstlendiği sorumluluğun gereği olarak, Korozyon Derneği bu alandaki gelişmelerin takipçisi olmayı görev sayacaktır. Dergimizin bu sayısında beton korozyonu üzerine Prof. Dr. Fevziye Aköz ün hazırladığı tanıtıcı bir makale ile betonarme yapıların korozyona karşı korunmasında katodik koruma uygulamalarını yansıtan çok kareli bir sunuyu okuyucularımızın incelemesine sunuyoruz. En içten esenlik ve başarı dileklerimizle! Basım Tarihi: Ağustos 2012 with Kurt Schwabe award given by European Corrosion Federation to shining young scientists with their distinguished contributions in corrosion science and engineering! On behalf of Corrosion Association, we sincerely congratulate Assoc. Prof. Ramazan Solmaz due to such significant success, which is also a source of honor for the corrosion community of our country. We share the reason of the award in this issue of our journal by announcing it in EFC-2012 April E-bulletin. In addition, you can also find Dr. Solmaz s curriculum vitae, a picture and his paper entitled Investigation of adsorption and inhibitive effect of 2-mercaptothiazoline on corrosion of mild steel in hydrochloric acid media published in 2008 on Electrochemica Acta and awarded with the highest referred publication award. DANGER THREATENING REINFORCED CONCRETE STRUCTURES: CORROSION Disaster on the reinforced concrete bridge built over Çaycuma Filyos Creek, in which the bridge was collapsed on April 6, 2012 due to flooding waters and 15 citizens were killed, as well as the earthquakes which became more frequent and surrounded almost the entire country give alarm on the high levels! It is clear that the cost of ignoring corrosion factor in the design and construction of reinforced concrete structures will get heavier on the shoulders of our nation. We, as the Corrosion Association, call our universities, research institute, nongovernmental organizations, and our state on duty! Such gap in the knowledge infrastructure of technical personnel to be charged with the design and construction of reinforced concrete structures should be filled in as soon as possible. Before else, our call is for our Universities and their relevant departments. We recommend and expect that our departments providing engineering and architecture programs should be fortified with courses and researches on corrosion. Basing on its foundation purposes and the responsibility it assumed, Corrosion Association considers its duty to follow up developments in this field. In this issue of our journal we share a multi pictured presentation reflecting the cathodic protection applications in protecting reinforced concrete structures against corrosion with an introductory article on corrosion of concrete composed by Prof. Dr. Fevziye Aköz. With sincere wishes of success! Date of Printing: August 2012

5 Doç. Dr. Ramazan SOLMAZ a Kurt Schwabe ödülü Bu yıl Kurt Schwabe ödülü Bitlis Üniversitesi Fen-Edebiyat Fakültesi Kimya Bölümü öğretim üyesi Doç. Dr. Ramazan Solmaz a verildi. Dr. Solmaz Fiziko-Kimya Ana Bilim Dalı ve Bitlis Üniversitesi Biyoteknoloji Araştırma ve Uygulama Merkezi nin başkanlıklarını yürütüyor. Dr. Solmaz korozyon bilimi ve korozyondan korunma dallarında gerçekleştirdiği seçkin katkıları ile birçok ödüle layık görülmüş değerli bir bilim adamıdır. Kısa sayılabilecek bir süre içinde uluslar arası dergilerde yayınladığı makale sayısı 31 e ulaşmıştı. Bunlardan pek çoğu sürekli atıf alan yayınlar arasındadır. Dr. Solmaz ISRN Corrosion dergisinin yayın kurulu üyesidir ve bugüne değin birçok bilimsel dergi için yayın değerlendirici olarak görev üstlenmiştir. Electrochemica Acta dergisinde yayımlanan The investigation of adsoption and imhibitive effect 0f 2-merceptathiozoline on the corrosion of mild steel başlıklı makalesi dönemi en fazla atıf alan makale ödülüne değer bulunmuştur. Halen Bingöl Üniversitesi Araştırma Fonu ve Türkiye Bilimsel ve Teknik Araştırma Kurumu tarafından desteklenen sekiz araştırma projesinde görevlidir. Dr.Solmaz ın ilgi alanı organik bileşiklerin karbon çeliği, bakır, alüminyum ve diğer metallerin çeşitli ortamlarda sergiledikleri korozyonu yavaşlatma etkisi, organik inhibitörlerin soğurulma ve inhibisyon mekanizmaları ve suyun elektrolizinde kullanılan elektrot malzemelerinin korozyonu üzerinde yoğunlaşmaktadır. Ödül bu yılın Eylül ayında İstanbul da, EUROCORR 2012 nin açılışında düzenlenecek seremoni ile Dr.Solmaz a verilecektir. (Kurt Schwabe ödülü Macaristan Korozyon Birliği (HUNKOR) tarafından ve Kurt Schwabe Vakfı nın desteği ile Prof.Dr.Kurt Schwabe nin onuruna yaşama geçirilmiştir. Ödül korozyon sorununa bilimsel ve teknik katkıları ile öne çıkan genç bilim insanlarına yayın temelinde yapılan değerlendirme sonucunda verilmektedir. Ödül bir madalya ve 500 Avro tutarında parasal katkıdan oluşmaktadır). The Kurt Schwabe Prize to Assoc. Prof. Dr. Ramazan Solmaz Assoc. Prof.Dr Ramazan Solmaz, Chemistry Dept., Science and Letters Faculty, Bingol University, Bingol, Turkey, has been chosen as this year s 2012 Kurt Schwabe Prize recipient. Dr. Solmaz is the current head of the Physical Chemistry division and the Director of the Biotechnology research and application center of his university. He is an outstanding scholar who has been awarded numerous prizes in recognition of his excellence in the research of corrosion science and corrosion protection. Within a relatively short time span of six years he has published 31 papers in international journals, many of which have been amongst the most cited articles on a continuous basis. He is a member of the editorial board of ISRN Corrosion, has reviewed numerous scientifi c journals and received the top cited article award for 2008 to 2009 for his paper entitled The Investigation of absorption and inhibitive effect of 2-mercaptothiazoline on the corrosion of mild steel in hydrochloric acid media published in Electrochemica Acta. He currently participates in 8 research projects supported by university research funds and the Turkish Scientifi c and Research Council. Dr. Solmaz s specialized fi eld o f corrosion research includes the investigation of corrosion inhibition effects of organic compounds on mild steel, copper, aluminum and other metals in various corrosive media, investigation of absorption and the corrosion inhibition mechanism of organic inhibitors, and investigation of the corrosion of electrode materials used for water electrolysis in operationmedia. Award will be presented to recipient at the opening ceremony of EUROCORR 2012 in Istanbul this September. (The Kurt Schwabe Prize, established by the Hungarian Corrosion Society HUNKOR with the fi nancial backing of the Kurt Schwabe Foundation, Hungary was established in honour of the late Prof. Kurt Schwabe. The award consists of a medal and the sum of 500 euro designated to a young scientist in recognition of his or her scientifi c and technical contribution to the fi eld of corrosion based upon publications).

6 INVESTIGATION OF ADSORPTION AND INHIBITIVE EFFECT OF 2-MERCAPTOTHIAZOLİNE ON CORROSION OF MILD STEEL IN HYDROCHLORIC ACID MEDIA* R. SOLMAZ* G. KARDAŞ* M. ÇULHA** B. YAZICI* M. ERBİL* ABSTRACT The inhibition effect of 2-mercaptothiazoline (2MT) on the corrosion behavior of mild steel (MS) in 0.5MHCl solutionwas studied in both short and long immersion times (120 h) using potentiodynamic polarization, electrochemical impedance spectroscopy (EIS) and linear polarization resistance (LPR) techniques. For long-term tests, hydrogen gas evolution (V H2 t) and the change of the open circuit potential with immersion time (E ocp t) were also measured in addition to the former three techniques. The surface morphology of the MS after its exposure to 0.5M HCl solution with and without M 2MT with the different immersion times was examined by scanning electron microscopy (SEM) and atomic force microscopy (AFM). The thermal stability of the inhibitor fi lmwas investigated by thermogravimetric analysis (TGA). The value of activation energy (E a ) for the MS corrosion and the thermodynamic parameters such as adsorption equilibrium constant (K ads ), free energy of adsorption ( G ads ), adsorption heat ( H ads ) and adsorption entropy ( S ads ) valueswere calculated and discussed. The potential of zero charge (PZC) of the MS in inhibited solution was studied by the EIS method, and a mechanism for the adsorption process was proposed. The results showed that 2MT performed excellent inhibiting effect for the corrosion of the MS. Finally, the high inhibition effi ciency was discussed in terms of adsorption of inhibitor molecules and protective fi lm formation on the metal surface. TGA results also indicated that the inhibitor fi lm on the surface had a relatively good thermal stability. 1. INTRODUCTION The adsorption of organic molecules at the metal/solution interface is of a great interest in surface science and can markedly change the corrosion resisting properties of metals. The protection of corroding surfaces prevents the waste of both resources and money during the industrial applications and it is vital for the extension of the lifetime of the equipment and limiting the dissolution of the toxic metals from the components into the environment. Therefore, the prevention from the corrosion of metals used in industrial applications is an important issue that must be dealt with. The use of inhibitors is one of the most practical methods for protecting against the corrosion and it is becoming increasingly popular. The organic molecules are recently used as corrosion inhibitors. The efficiency of these molecules is mainly dependent on their ability to be adsorbed on the metal surface, which results with the replacement of water molecules at a corroding interface 1. In recent years, there is a considerable amount of effort devoted to find novel and efficient corrosion inhibitors and sulphur and/or nitrogen containing molecules have been found to be effective corrosion inhibitors 2-6. The 2MT is a molecule that has practical applications in the plating solution of printed wiring board industry such as brightening and stabilization agents 7. The chemically modified 2MT was used for the purpose of the selective adsorption of the heavy metal ions and reported to be very selective to Hg(II) ions in aqueous solutions 8. A 2MT molecule has two sulphur atoms and one nitrogen atom as well as electrons which are assumed to be active centre of adsorption. The corrosion inhibition effect of 2MT has not been studied as corrosion inhibitor in details. Wang et al. 9 was studied 2MT as inhibitor for the corrosion of low carbon steel in phosphoric acid solution by weight loss method. However, Figure 1. The chemical structure of 2-mercaptothiazoline (2MT). * 2008 yılında Electrochemical Acta adlı dergide yayımlanan bu makale dönemi en fazla atıf alan makale olarak ödüllendirildi. Bu değerli katkıyı EFC Kurt Schwabe ödülünü kazanan Doç. Dr. Ramazan Solmaz ve birlikte çalıştığı bilim insanlarının ilgi alanını tanıtmak üzere okurlarımızın bilgi ve değerlendirmelerine sunuyoruz. 6

7 a detail study on the adsorption mechanism and inhibition effect of 2MT on the corrosion of MS has not been reported yet. The aim of this study is to report on the inhibition effect of 2MT on the corrosion behavior of MS in 0.5 M HCl solution in both short and long immersion times and clarify its inhibition mechanism. 2. EXPERIMENTAL 2.1 Field Data Collection The working electrode was a cylindrical disc cut from an MS rod with following chemical composition (wt); C (0.21%), Si (0.36%), Mn (1.25%), P (0.025%), S (0.046%), Cr (0.16%), Ni (0.16%), Cu (0.41%), Mo (0.017%), Sn (0.017%), Al (0.003%), V (0.081%) and Fe (remainder). The preparation of working electrode before measurements is the same as described before 10. The exposed surface area of the MS was 0.50 cm Test solutions The tests were performed in 0.5 M HCl solution and containing various concentrations of 2MT, whose chemical structure is given in Fig. 1. An aggressive solution (0.5 M HCl) was prepared by dilution of 37% HCl. The concentration range of the inhibitor employed was varied from M to M. All the test solutions were prepared from analytical-grade chemical reagents in distilled water without further purification. For each experiment, a freshly prepared solution was used. During the experiments, the test solutions were opened to air. For potentiodynamic polarization measurements, the test solutions were continuously stirred using a magnetic stirrer while all the others were performed under un-stirring conditions. The solution temperature was thermostatically controlled at a desired value. 2.3 Electrochemical measurements A CHI 604 model computer controlled electrochemical ana lyzer (serial number: 6A721A) was used for the electrochemical measurements. A double-wall one-compartment cell with a threeelectrode configuration was used. A platinum sheet (with 2 cm 2 surface area) and Ag/AgCl electrode were used as the auxiliary and the reference electrodes, respectively. All potential values were referred to this reference electrode. The working electrode was first immersed in the test solution and after establishing a steady state open circuit potential, the electrochemical measurements were Table 1. Electrochemical parameters for the MS determined from polarization measurements in 0.5M HCl and containing M 2MT solutions C inh (M) E corr (V) I corr (A cm 2 )( 10 5 ) W L (g m 2 h 1 ) IE% Blank performed. The polarization curves were potentiodynami cally obtained in the potential ranges from 0.90 V to 0.10 V with a scan rate of V s 1. The EIS experiments were conducted in the frequency range of 100 khz to Hz at an open circuit potential by applying alternating current signal of V peak-to-peak. The linear polarization measurements were carried out by record ing the potential ±0.010 V around open circuit potential at a scan rate of V s 1. The polarization resistance (R p ) was determined from the slope of the obtained current potential lines. In order to investigate the mechanism of the inhibition and calculate the activation energy of the corrosion process, the polar ization curves were obtained at various temperatures (25 55 o C) in the absence and the presence of M 2MT. To determine the potential of zero charge of the MS, the impedance of the MS was determined at different potentials in M 2MT containing 0.5 M HCl solutions. The corrosion behavior of the MS in inhibited and uninhibited solutions with immersion time was also performed with immer sion time up to 120 h. For this purpose, the potentiodynamic polarization, EIS, LPR, PZC, the hydrogen gas evolution (V H2 t) and the change of open circuit potential with immersion time (E ocp t) were utilized. During the long-term tests, the working electrode was immersed in a beaker which contains 200 ml test solution. After different immersion times, electrochemical measurements were performed under the un-stirring conditions. In the hydro gen gas evolution measurements, a burette was filled with 0.5 M HCl solution and turned over the working electrode. The initial volume of air in the burette was recorded and the volume of H 2 gas evolved from the corrosion reaction was monitored by the vol ume change in the level of the solution as a function of time. The same experiment was repeated in the presence of M2MT. The long-term tests were carried 7

8 Figure 2. Polarization curves for MS recorded after 1 h (a) and 120 h (b) of exposure time in 0.5M HCl solution free ( ) and containing ( ), ( ) and M ( ) 2MT. out at room temperature ( 25 o C) under un-stirring conditions. 2.4 SEM and AFM studies In order to examine the changes in surface morphology of the electrodes covered with a thin film of 2MT, the electrodes were immersed in 200 ml 0.5 M HCl and M 2MT containing 0.5 M HCl solutions. After 24 h and 120 h waiting time, the electrodes were removed from the cells, washed with distilled water and dried. The SEM images were taken using a Carl Zeiss Evo 40 SEM instrument at high vacuum and 10 kv EHT, AFM images were taken with Park SYSTEMS using non-contact mode. 2.5 Thermal stability of surface film A series of electrodes were immersed in 0.5 M HCl solution containing M 2MT for a period of 120 h. After this time period, the specimens were taken out, washed with distilled water and dried. The organic thin film was mechanically removed from the electrode surfaces and its thermal stability was tested. The thermal analysis experiments were performed under the nitrogen atmosphere using Pyriss Diamond TG/DTA Perkin-Elmer thermal analysis and Pyriss 7.0 data-processing system at a heating rate of 20 o Cmin 1 over a temperature range of o C. 3. RESULTS AND DISCUSSION 3.1 Potentiodynamic polarization measurements The potentiodynamic polarization curves of the MS in 0.5 M HCl solution with various concentrations of 2MT after 1 h of immersion time are presented in Fig. 2a. The related electrochemical parameters, i.e., corrosion potential (E corr ), corrosion current density (i corr ), weight loss (W L ) and inhibition efficiency (IE%) values were calculated from these Figure 3. The Nyquist (a) and log (freq) log (Z) plots (b) for the MS electrode obtained in 0.5MHCl solution free ( ) and containing ( ), ( ) and M ( ) 2MT. 8

9 Figure 4. The potential distributions on the metal/solution interface (a), the resistances related double layer (b), and proposed electrical equivalent circuit diagram for blank solution (c). OHP: Outer Helmholtz plane; C dl : double layer capacitance; R s : solution resistance; R ct : charge transfer resistance; R d : diffuse layer resistance; R a : resistance of accumulated species (corrosion products, any existing molecules or ions, etc.); R p : polarization resistance. Figure 5. Schematic representation of metal/inhibitor/solution interface (a) and proposed equivalent electrical circuit diagram for EIS results of the MS in inhibited solutions (b). C f : fi lm capacitance; R f : fi lm resistance. curves and listed in Table 1. The inhibition efficiency IE% was calculated from polarization measurements according to the relation; ( icorr ) i corr IE(%) = 100 (1) i corr where i corr and i are the uninhibited and the inhibited corrosion current densities, respectively. corr These values were obtained by the extrapolation of the current potential lines to the corresponding corrosion potentials. The weight loss was calculated theoretically with the help of the corrosion current values. It is clear from Fig. 2a that, as would be expected, both anodic metal dissolution of iron and cathodic hydrogen evolution reaction were inhibited after the addition of 2MT to the aggressive solu tion. The inhibition of these reactions is more pronounced with the increasing inhibitor concentration 9

10 Figure 6. Nyquist plots for the MS in HCl solution ( ) and containing MT ( ) after different exposure times (inset shows the Nysuist plot of blank solution). while the corrosion potential values are nearly remained the same. These results suggest that 2MT can be classified as mixed type corrosion inhibitor. The cathodic current potential curves (Fig. 2a) give rise to parallel lines indicating that the addition of 2MT to the 0.5 M HCl solution does not modify the hydrogen evolution mechanism and the reduc tion of H + ions at the MS surface takes place mainly through a charge transfer mechanism. The inhibitor molecules are first adsorbed onto the MS surface and, therefore, impedes by merely blocking the reaction sites of the MS surface. In this way, the surface area available for H + ions is decreased while the actual reaction mech anism remains unaffected 11. A higher coverage of the inhibitor on the surface was obtained in solutions with the higher inhibitor concentrations. The presence of defects on the metal surface (1 θ) permits a free access of H + ions to the MS surface 12. In anodic current potential curves at potentials higher than V, the inhibition effect of 2MT on the iron dissolution reaction reduces. This potential is usually defined as the desorp tion potential, which means that the inhibition mode of inhibitor depends on the electrode potential. This behavior may be the result of a significant dissolution of iron, leading to desorption of the inhibitor film from the metal surface. In this case, the desorp tion rate of the inhibitor is higher than its adsorption rate 13. The observed phenomenon is generally described as the corrosion inhibition of the metal with the formation of a protective layer of adsorbed species at the metal surface The potentiodynamic polarization curves for the MS in 0.5 M HCl solution and with the addition of M 2MT were also obtained after 120 h of immersion time, and the recorded plots are presented in Fig. 2b. It is clear from these plots that both the anodic and cathodic current values were considerably increased in uninhibited 0.5 M HCl solution when compared with the ones that obtained after 1 h of exposure time. This observation can be explained with an increase in surface area of the MS because of the excess dissolution of iron. It is evident that the corrosion cur rent density of the MS is much smaller when 2MT is added to the aggressive solution ( A cm 2 and A cm 2 after 120 h in uninhibited and inhibited solu- 10

11 Figure 7. log (freq) log (Z) plots for MS in 0.5M HCl solution free ( ) and containing M 2MT ( ) after different exposure times. tions, respectively), and the corrosion potential is shifted by V in a cathodic direc tion. A decrease in the slope of cathodic current potential line (from 140 to 123 V dec 1 ) and an increase in the slope of the anodic current potential line were observed in the inhibited solu tion when compared to those of the short immersion times. This indicates the modification of anodic and cathodic reaction mech-anisms in inhibited solution with the immersion time. After this time period, the inhibition efficiency was calculated using Eq. (1) and found to be 99.3%. The formation of the surface inhibitor film on the MS surface provides considerably proper protection for the MS corrosion. This film reduces the active surface areas exposed to the corrosive medium and delays the hydrogen evolution and the iron dissolution. In addition, it must be emphasized that the high value of IE was obtained merely on the basis of strong increase of the current density value after 120 h in the blank solution Electrochemical impedance spectroscopy Nyquist plots and the representative Bode diagrams for the MS electrode in 0.5 M HCl solution and containing various concentra tions of 2MT after 1 h of immersion time are given in Fig. 3a and b, respectively. It is clear from these figures that in uninhibited solution, Nyquist plot yields a slightly depressed semi circular shape and only one time constant was observed in Bode format. This indicates the corrosion of the MS in the absence of inhibitor and mainly controlled by a charge transfer process 14,16. In the evaluation of Nyquist plots, the difference in real impedance at lower and higher frequencies is commonly considered as a charge transfer resistance. The charge transfer resistance must be corresponding to the resistance between the metal and OHP (outer Helmholtz plane). The contribution of all resistances correspond to the metal/solution interface, i.e., charge transfer resistance (R ct ), diffuse layer resis tance (R d ), accumulation resistance (R a ), film resistance (R f ), etc. must be taken into account. Therefore, in this study, the difference in real impedance at lower and higher frequencies is considered as the polarization resistance (R p ) The addition of 2MT to the aggressive solution leads to a change of the impedance diagrams in both shape and size, which a depressed semicircle at the 11

12 Table 2. Electrochemical parameters for MS corresponding to the EIS and LPR data in 0.5M HCl free and containing M 2MT solutions Table 3. The polarization resistance and percentage inhibition effi ciency values corresponding to the EIS and the LPR data in 0.5M HCl and containing M 2MT solutions C (M) EIS LPR R p () IE% R p () IE% Blank t (h) Blank 2MT EIS LPR EIS LPR R p () R p () R p () IE% R p () IE% high frequency part of the spectrum was observed and a second time constant appeared at low frequency region. The first capacitive loop appearing at high frequency region was attributed to the charge transfer resistance and the diffuse layer resistance, the second one at low frequencies related to the adsorption of inhibitor molecules on the metal surface 19 and all other accumulated kinds at the metal/ solution interface (inhibitor molecules, corrosion products, etc.) 6. As seen from Fig. 3a, the Rp values increased with the 2MT concentration, which can be attributed to the formation of a pro-tective overlayer at the metal surface, which becomes a barrier for the mass and the charge transfers. The double layer can be represented by the electrical equiva lent circuit diagrams to the model metal/solution interface. The corresponding electrical equivalent circuit model for the MS in uninhibited solution is given in Fig. 4c with a schematic represen tation of the potential distributions on the metal/solution interface (Fig. 4a) and the resistances related to the double layer (Fig. 4b) 17. According to Fig. 4, the polarization resistance includes the charge transfer resistance, the diffuse layer resistance and all the other accumulated kinds of ions, corrosion products, etc. at metal/solution interface. The charge transfer resistance must be corresponded to the resistance between the metal and OHP (outer Helmholtz plane). All the other resistances must be considered as the simple resistance on the current crossing away 18.Inthe case of the inhibited solutions, related electrical equivalent cir cuit model is given in Fig. 5b with a schematic representation of metal/solution interface (Fig. 5a). In the literature, a similar repre sentation was proposed for polymer coated MS electrode 20. The values of polarization resistance and related percentage inhibition efficiency values, which were determined from the EIS, are listed in Table 2. The polarization resistance values were also determined from the LPR technique and given in the same table with corresponding inhibition efficiencies. The inhibition efficiency was calculated from the polarization resistance using the following formula; ( ) R p R p IE % = 100 (2) R p where Rp and Rp are uninhibited and inhibited polarization resistances, respectively. EIS provides a rapid and convenient way to evaluate the performance of the organic-coated metals 21 and has been widely used for investigation of protective properties of organic inhibitors on metals. It is particularly a useful technique to follow evolution of inhibitor metal system over time. It does not disturb the double layer at the metal/ solution interface 17. Therefore, more reliable results can be obtained from this technique. From longer immersion times, it was possible to characterize the surface layer modification, i.e., formation and growth of inhibitor film 22. For this purpose, the impedance measurements for the MS in uninhibited and inhibited 0.5 M HCl solution with the addition of M 2MT after different immersion times were also performed. The obtained results are given in Figs. 6 and 7 in Nyquist and Bode representation, respectively. After 4 h, the polarization resistance for the MS in uninhibited solution was reduced to 40 from 44.In the presence of 2MT, the shape of diagram changed compared to the ones obtained after the 1 h of immersion time. The Nyquist plot includes only one slightly depressed semi circle and the R p value is larger. This indicates the formation of a compact and protective thin film on the MS surface. In this case, the MS corrosion could only take place on the free surface of the me- 12

13 Figure 8. The change of hydrogen gas evolution on the MS electrode with exposuretime in 0.5M HCl ( ) and containing M2MT ( ) solutions. Figure 10. Arrhenius plots for the MS electrode in 0.5M HCl ( ) and containing M2MT ( ) solutions. tal and/or within the pores; if the metal surface is fully covered, the corrosive species, i.e., dissolved oxygen, chloride ions, must diffuse along these pores to interact with the metal surface 20. After 24 h (Fig. 6b), the diameter of the semicircle recorded in the presence of the inhibitor increased significantly as compared to shorter exposure times, which indicated the continuous growth of the surface film and the approach in the perfect coverage of the surface film on the metal. The growth of this layer enhanced the corrosion resistance of the metal. After this time period, the Nyquist plot for the inhibited solution presents an increase of the phase angle (θ-11.5 O at Hz) indicating that the mass transport is limited by the surface inhibitor film and accumulated species. In contrary to the inhibited solution, the polarization resistance of the MS in blank solution was reduced with the exposure time. After 120 h (Fig. 6d), a slight decrease in the R p value of the MS in inhibited solution was observed, which may be due to the formation of some defects on the film leading to the access of aggressive ions to the metal/ inhibitor interface. The values of both polarization resistance and corrosion inhibition efficiency values (IE%) corresponding to the EIS and the LPR data as being associated over 120 h immersion times are given in Table 3. The IE% values obtained from the EIS are comparable and run parallel with those obtained from the LPR and the potentiodynamic polarization measurements. It is clear from Table 3 that a strong decrease of the R p value in blank solution was obtained with the increased immersion time. However, the R p value in the inhibited solution increases up Figure 9. The change of open circuit potential with immersion time in 0.5M HCl ( )and containing M2MT ( ) solutions. Figure 11. Langmiur adsorption plot for the MS electrode in 0.5M HCl containing different concentrations of 2MT. 13

14 to 24 h, and then tends to decrease. Because of a strong decrease in the R p value for uninhibited 0.5 M HCl solution compared to the inhibited one, a high IE value was calculated after 120 h of exposure time. 3.3 Hydrogen gas evolution measurements The gasometric techniques provide a rapid and reliable means for the assessment of the inhibitive capabilities of inhibitors on the MS corrosion in acidic media. The relative speed and effectiveness of the gasometric techniques as well as their suitability for in situ monitoring, any perturbation by an inhibitor with respect to gas evolution in metal/solution systems has been established in the literature The volume of H 2 gas evolved from the corrosion reaction in both inhibited and uninhibited 0.5 M HCl solutions as a function of exposure time at 24 h intervals and the obtained data are presented in Fig. 8. As can be seen, the rate of H 2 evolution is small at the beginning of the reaction, and after a certain time, it increases remarkably because of the increased surface area of the MS as a result of the excess iron dissolution. It is clear from Fig. 8 that, the rate of H 2 evolution was considerably reduced after the addition of 2MT to the aggressive media indicating that the inhibitor molecules adsorb strictly onto the MS surface and block the electrochemical reaction efficiently through decreasing the available surface area. After 120 h of immersion time, 146 ml cm 2 H 2 gas evolved in 0.5 M HCl solution, whereas only 0.8 ml cm 2 hydrogen gas evolved in M 2MT containing 0.5 M HCl solution per unit area of the MS. 3.4 Change of open circuit potential with immersion time Since they can provide important insights about the corrosion behavior of metals as well as the porosity of the surface films, the variation of the open circuit potential of the MS as a function of immersion time (E ocp t) was measured against Ag/AgCl reference electrode in 0.5 M HCl solution containing M 2MT over 120 h. The obtained data are presented graphically in Fig. 9. As seen, in blank solution, the E ocp value of the MS shifts towards more positive potentials continuously up to 24 h and after this time period it is nearly stable around V (Ag/AgCl). The addition of M 2MT to the 0.5 M HCl solution produce a considerably nobler E ocp value and tends to posses more cathodic values with the increasing immersion time. After 24 h, more negative E ocp values were measured for the inhibited solution than in uninhibited solution and after this time, they tend to shift towards cathodic potentials slightly up to 120 h. The obtained results Scheme 1 clearly indicate the adsorption of 2 MT molecules on the cathodic sites of the metal surface, which blocks these areas efficiently. Figure 12. The plot of Cdl vs. applied electrode potential in 0.5M HCl containing M 2MT solution. 3.5 Effect of temperature In order to calculate the activation energy of the corrosion process and investigate the mechanism of inhibition, potentiodynamic polarization measurements were performed in the temperature range of o C in the absence and presence of M 2MT solutions. The dependence of the corrosion rate on temperature can be expressed by the Arrhenius equation; i corr = A exp ( Ea RT ) (3) 14

15 where i corr is corrosion current, A is a constant, Ea the activation energy of the metal dissolution reaction, R is the gas constant and T is the temperature. The Ea values were calculated from the Arrhenius plots (Fig. 10) and found to be kj mol 1 and kj mol 1 for the corrosion process in the absence and presence of 2MT, respectively. The increase in activation energy after the addition of the inhibitor to the 0.5 M HCl solution indicates that physical adsorption (electrostatic) occurs in the first stage The higher E a value in the inhibited solution can be correlated with the increased thickness of the double layer, which enhances the activation energy of the corrosion process. 3.6 Adsorption isotherm and thermodynamic consideration The adsorption on the corroding surfaces never reaches the real equilibrium and tends to reach an adsorption steady state. However, when the corrosion rate is sufficiently small, the adsorption steady state has a tendency to become a quasi-equilibrium state. In this case, it is reasonable to consider the quasi-equilibrium adsorption in thermodynamic way using the appropriate equilibrium isotherms 27. The adsorption isotherms can give important information on the interaction of inhibitor and metal surface. Langmuir, Temkin, Bockris-Swinkels, Flory -Huggins and Frumkin adsorption isotherms were tested in order to find the best suitable adsorption isotherm for adsorption of 2MT on the MS surface from 0.5 M HCl solution. Langmuir adsorption isotherm, which is given by Eq. (4) was found more suitable with an average correlation coefficient of and the slope of (Fig. 11). (Langmuir adsorption isotherm was plotted using data of the EIS, the potentiodynamic polarization measurements and the LPR techniques and average values of thermodynamic parameters of the adsorption process were given). C (inh) = 1 K (ads) + C (inh) (4) Table 4. Thermodynamic values and the Antropov s rational corrosion potentials of the MS in 0.5M HCl containing M 2MT solution after different immersion times t (h) E r (V) K ads (M 1 ) G ads (kj mol 1 ) where C(inh) is inhibitor concentration, θ is the degree of the coverage on themetal surface and K ads is the equilibrium constant for the adsorption desorption process. The value of equilibrium constant, Kads calculated from the reciprocal of the intercept of isotherm line as M 1. The high value of the adsorption equilibrium constant refl ects the high adsorption ability of this inhibitor on MS surface. The free energy of the adsorption of inhibitor onms surface can be evaluated with the following equation; G ads = RT ln (55.5K ads ) (5) From Eq. (5), G ads was calculated as kj mol 1. The negative value of LGads indicate spontaneous adsorption of the 2MT on the MS surface 3 and also the strong interaction between inhibitor molecules and the metal surface 28. The value of LGads is less than 40 kj mol 1 is commonly interpreted with the presence of physical adsorption by the formation of an adsorptive film with an electrostatic character The heat of adsorption (Q ads ) and the entropy value of the inhibitor adsorption ( S ads ) was calculated as described in the literature and found to be 9.33 kj mol 1 and J mol 1 K 1, respectively. The negative sign of H ads indicates that the adsorption of 2MT on the MS surface from 0.5 M HCl solution is an exothermic process. The adsorption process of 2MT onto MS surface includes, at least, two steps: the adsorption of 2MT molecules onto MS surface and simultaneous desorption of some hydration water from the MS surface. The former process is expected to cause a decrease in randomness, thus in S ads. The later process could cause some increase in disorderness. The obtained entropy value seems to be in contrast to that normally accepted in the adsorption phenomenon. While the adsorption of organic molecules is generally exothermic with decrease in entropy, the contrary occurs for the desorption of water molecules. The thermodynamic values obtained are the algebraic sum of those of the adsorption of organic molecules and desorption of water molecules. Therefore, the positive value of S ads related to substitutional adsorption can be attributed to the increase in the solvent entropy and to more positive water desorption entropy 32. The positive value of S ads was also interpreted by the increase of disorder due to desorption of more water molecules from the metal surface by one inhibitor molecule

16 l f h l d d ff d d h d l b d l f d 2 Figure 13. Nyquist plots for the MS electrodes at different anodic and cathodic over potentials obtained in 0.5M HCl free and containing M 2MT l solutions. 3.7 The potential of zero charge and inhibition mechanism It is well known that organic inhibitors generally act through adsorption on the metal surface. Their adsorption depends mainly on the surface charge of the metal, the charge or dipole moment of inhibitor, and the adsorption of other charged ionic species 34. The surface charge of metals can be determined by the comparison of open circuit potential with the respective potential of zero charge (PZC). In order to gain more information about the surface charge of the MS, the EIS technique was used to define the PZC of the MS in the inhibited 0.5 M HCl solution with the addition of M 2MT. The dependence of double layer capacitance (C dl ) on the applied potential after 4 h of immersion time is given graphically in Fig. 12. As seen, the obtained curves show a parabola with a minimum at V (Ag/AgCl), which can be called the PZC of the MS in 0.5 M HCl solution containing M 2MT 35. The open circuit potential of the MS in the same conditions is V (Ag/AgCl). The difference, E r = E ocp E pzc = V, where Er is the Antropov s rational corrosion potential 5 is positive, which means the metal surface is positively charged at the open circuit potential after 4 h of exposure time. Based on the PZC experiments, several adsorption mechanism can be proposed for the 2MT molecules on the MS surface. The following mechanism is proposed for the corrosion of the MS in uninhibited and inhibited HCl solutions (Scheme 1). In hydrochloric acid solution without inhibitor, the mechanism of the anodic dissolution reaction of iron follows the reaction path-wayfromatod (a d)

17 In the presence of M2MT, the value of the PZC, which is obtained after 4 h of immersion time, indicates that positive excess charge is carried on the MS surface. It is well known that the chloride ions have a small degree of hydration, and due to specific adsorption, they bring an excess negative charge towards the solution side of metal attracting most of the cations 37. The 2MT molecules exist as protonated through nitrogen atoms in HCl solution and it is in equilibrium with the corresponding molecular form, whose pka value was reported to be 11± The protonated inhibitor molecules could be adsorbed on the metal surface via chloride ions, which form interconnecting bridges between the positively charged metal surface and protonated organic cations Thus, a close packed triple layer will form on the metal surface, which reduces the mass and charge transfers. Therefore, it can be hypothesis that the reaction pathway is through a to e, which have the rate constant k2. If this is the case, the rate constant k2 must be much more larger than k4(k2» k4) and the reaction pathway (a e) is more favored than (a b). The surface charge of the MS surface was also determined after longer immersion times. The obtained E r values are presented in Table 4. While the E r potential was found to be decreasing with the increased of exposure time, whereas its sign is still positive up to 24 h. This means a gradual decrease in positive charge on MS surface towards solution side. After 120 h, the value of E r was determined as V suggesting that the metal surface was negatively charged. After the first electrostatical adsorption of the inhibitor molecules via formerly adsorbed chloride ions, the 2MT molecules would directly be adsorbed onto the metal surface. The gradually replacement of positively charged inhibitor molecules with the chloride ions decreases the positive excess charge on MS surface and finally creates a negative excess charge. When this is the case, the reaction mechanism is changed and the reaction step proceeded from (FeCl Inh + )ads to (FeInh + )ads as a new reaction pathway having the rate constant k3 (e f). The rate constant k 3 related to the forming (FeInh + )ads (k 3 ) must be bigger than k 2 as well as k 4. Thus, for longer immersion times, it can be hypothesized that the reaction pathway is through a to f (a f). The change in reaction mechanism is also supported by the result of the potentiodynamic polarization measurements. Figure 14. Nyquist plots for the MS electrodes at different anodic and cathodic over potentials obtained in 0.5M HCl free and containing M 2MT solutions. 17

18 The cathodic hydrogen evolution reaction may be given as follow; Fe + H + (FeH + ) ads (FeH + ) ads + e (FeH) ads (FeH) ads + H + + e Fe + H 2 (6) (7) (8) The protonated 2MT molecules are also adsorbed at cathodic sites in competition with hydrogen ions that going to reduce H2 gas evolution 36. In order to support the proposed reaction mechanism, we have also determined the change in the adsorption equilibrium constant and the free energy of the adsorption as a function of immersion time using the LPR technique, and the data is listed in Table 4. The variation of both Kads and LGads values with immersion time indicates the change in mechanism of the inhibitor action. An increase in both Kads and LGads values, which support better adsorption of the inhibitor molecules on the metal surface, were found after 120 h. After this time period, the value of LGads reached kj mol 1 indicating the contribution of chemical adsorption. In addition to the physical adsorption, the adsorption of 2MT can occur directly on the basis of donor acceptor interactions between electrons and N atoms of the neutral species as well as electrons of cationic species and the vacant d orbitals of iron. It has been reported that the adsorption of the heterocyclic compounds occurs with the aromatic rings some times parallel but mostly normal to the metal surface 33. The orientation of molecules could be dependent on the ph and/or electrode potential. However, more work should be completed to confirm the above arguments 33. In the case of parallel adsorption of inhibitor molecules, the steric factors also must be taken into consideration. If the steric factors are in place, the chemical adsorption may be occurring through the molecular form. The increase in K ads and G ads with exposure time values support the contribution of the chemical adsorption with increasing exposure time 40. The anodic dissolution and the cathodic reduction reactions were investigated both in blank and M 2MT containing 0.5 M HCl solutions by the EIS method at different anodic and cathodic over potentials, which were previously determined from the polarization curves. The data are presented in Nyquist representation and given in Fig. 13 with the polarization plots, which were obtained after 1 h of immersion time. As can be seen from Fig. 13, in the cathodic range, only one capacitive loop was obtained in blank solution at 200 mv over potential indicating that at this potential the reduction of H + ions was completely charge transfer controlled. The polarization resistance of the MS in the blank solution at 200 mv was 5.6. It can be concluded that, in the inhibited solution, the reduction mechanism does not change and the Nyquist plot of the MS in inhibited solution at 200 mv also contains only one capacitive loop indicating that reduction reaction is charge transfer controlled. At this over potential, the R p of the MS was relatively larger (155 ) when compared to one that obtained in blank solution. These results show that the inhibitor molecules are adsorbed on the MS surface and the surface area available for H + ions is decreased. In anodic range, a different behavior was observed. At +100 mv, Nyquist plot of the MS in the blank solution contains two time constants. The first loop appeared at high frequencies was attributed to the charge transfer resistance, the second loop at the low frequencies may be due to accumulated corrosion products at metal surface, which hinders ion diffusion. A straight line was observed at the high frequencies and a second capacitive loop was observed at low frequencies for M 2MT containing 0.5 M HCl solution at +100 mv. The first loop was attributed to the charge transfer resistance and the second loop to the film resistance. The Rp value of the MS in inhibited solution at +100 mv was 370 and larger than that of the blank solution (27 ). At the higher anodic over potentials (+300 mv), a capacitive loop was observed at the high frequencies and followed an inductive loop was appeared at low frequencies in blank solution. Such inductive loops at low frequencies were commonly attributed to the relaxation process 41. It is clear from Fig. 13 that a small inductive loop at low frequencies also appeared in the presence of the inhibitor. This observation shows that a relaxation of the surface inhibitor film takes place at more positive potential. This behavior may be the result of significant dissolution of iron leading to desorption of the inhibitor film from the metal surface. 3.8 SEM and AFM studies The SEM images of the MS surfaces exposed to 0.5 M HCl without and with the M 2MT for 24 h and 120 h are given on Fig. 14. The inspection of Fig. 14a, which is the micrograph of the MS surfaces exposed to 0.5 M HCl solution for 24 h, reveals clear pits with a small size distribution over the surface of the MS. The polishing stretches 18

19 Figure 15. The AFM images of MS surfaces after exposing to 0.5M HCl solution for 24 h (a), 120 h (b) and exposing to 0.5M HCl containing M 2MT solution after 24 h (c) and 120 h (d). were also visible on the surface. With the increasing exposure time (120 h), the specimen surface was strongly damaged in the absence of the inhibitor with the increased number and the depth of the pits (Fig. 14b). Fig. 14c shows the SEM images of the MS surface exposed to 0.5 M HCl with the addition of M 2MT for 24 h. There are no pits and cracks observed in the micrograph expect polishing lines. The metal surface was fully covered with the inhibitor molecules and a protective inhibitor film was formed. The surface image of the MS exposed to inhibited solution for 120 h is shown in Fig. 14d. As seen, the inhibitor molecules covered only active sites of the MS and some regions are not covered. It is interesting to note that there is not any sign of damages on these uncovered inhibitor free zones. Therefore, it can be concluded that the high inhibition efficiency of 2MT after longer immersion times may be due to the adsorption of inhibitor molecules on the active sites of the MS surface which means that, after the longer immersion time, the adsorption is more chemical than physical one. AFM is a powerful technique to investigative the surface mor-phology at nano-to micro-scale and has become a new choice to study the influence of inhibitors on the generation and the progress of the corrosion at the metal/solution interface. The threedimensional AFM images of the MS surface exposed to 0.5 M HCl with and without M 2MT solutions for 24 h and 120 h are shown in Fig. 15. The surface image of (Fig. 15a) the MS exposed to 0.5 M HCl solution for 24 h shows the main characteristic of the pitting corrosion. With the increased exposure time (120 h), both the width and the depth of the pits were increased (Fig. 15b). The image of the MS surface exposed to 0.5 M HCl solution with the addition of M 2MT for 24 h is given in Fig. 15c. It clearly evident that, the surface is more uniform than the surface in the absence of the inhibitor except some hallows structures. The polishing lines were also visible on the surface. After 120 h, the inhibitor molecules were adsorbed to the active sites and a smoother surface (Fig. 15d) was observed when compared to the surface treated with uninhibited 0.5 M HCl solution (Fig. 15b). 3.9 Thermal stability of the surface film The thermal stability of the surface inhibitor film is very important for their applications. Acid pickling of steel is usually carried out at elevated tempera- 19

20 Figure 16. TGA curves of 2MT removed from electrode surface (a) and pure 2MT compound (b). tures up to 60 o C in HCl and up to 90 o C in H 2 SO 4 solutions 5. Therefore, the organic inhibitors are expected to be chemically stable to provide a high protective efficiency under the conditions mentioned above. The thermogravimetric analysis (TGA) of inhibitor film removed mechanically from the MS surface was tested and the obtained TGA curve is shown in Fig. 16a. For comparison, the TGA of the pure organic compound was also performed and given in Fig. 16b. A comparison of TGA curves for pure 2MT compound and that of inhibitor film removed from the metal surface reveal the differences in thermal events. As seen from Fig. 16b, the pure 2MT compound shows only one sharp step weight loss which starts at 170 o C, whereas the TGA curve of 2MT, which removed from the MS surface, shows three-step weight loss. The initial weight loss up to 170 o C could be attributed to the loss of moisture and dopands 42,43. Between 200 o C and 400 o C a slower weight loss occurs due to thermal degradation of 2MT. The last weigh loss step displayed between 400 o C and 440 o C may be corresponding to the metal inhibitor complex degradation. The remaining weight cor-responds to the iron metal. From these results, it can be concluded that the surface inhibitor film possesses relatively good thermal stability. 4. CONCLUSIONS The adsorption and inhibition effect of 2MT on the corrosion behavior of the MS in 0.5 M HCl was studied in both short and long immersion times (up to 120 h) using different techniques. The following points can be emphasized; 1. The obtained results showed that 2MT performed perfect inhibition efficiency for the corrosion of the MS in 0.5 M HCl solution and the inhibition efficiency was more pronounced with inhibitor concentration and exposure time. The high inhibition efficiency of 2MT was attributed to the adherently adsorption of the inhibitor molecules on the MS surface, and a protective film formation. 2. The potentiodynamic polarization curves indicated that 2MT inhibits both anodic metal dissolution and also cathodic hydrogen evolution reactions. 3. The adsorption of 2MT molecules on the metal surface from 0.5 M HCl solution obeys Langmiur adsorption isotherm. The high value of adsorption equilibrium constant suggested that, 2MT is strongly adsorbed on the MS surface. The negative sign of the G ads and H ads indicate that the adsorption process is spontaneous and exothermic. 4. The increase in activation energy after the addition of 2MT to the 0.5 M HCl solution and the value of free energy of the adsorption indicated that the adsorption is more physical than the chemical adsorption (after 1 h of exposure). However, both G ads and K ads values were found to be increased with exposure time suggested that the adsorption mechanism tends to be chemical with the immersion time. 5. The analysis of the AFM and SEM images was showed the corrosion of the MS is mainly through pitting and the addition of inhibitor to the aggressive solutions results through the formation of a protective film on MS surface. 6. The TGA results were shown relatively good thermal stability of the surface inhibitor film in a typical temperature range of working conditions of pickling. ACKNOWLEDGEMENTS This study has been financially supported by Cukurova University research fund. The authors are greatly thankful to Cukurova University research fund. The authors also thank The Scientific and Technical Research Council of Turkey (TUBITAK) for financial support. We also would like to acknowledge Prof. Dr. Osman Serindağ for thermal analysis experiments. REFERENCES 1. J.O M. Bockris, A.K.N. Reddy, Modern Electrochemistry, vol. 2, Plenum Publishing Corporation, 227West 17th, Street, New York, H. Keleş, M. Keleş, İ. Dehri, O. Serindağ, Colloids Surf. A: Physicochem. Eng. Aspects. 320 (2008) L. Tang, X. Li, L. Li, G. Mu, G. Liu, Mat. Chem. Phys

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