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Öğe Silica gel-immobilized 5-aminoisophthalohydrazide: A novel sorbent for solid phase extraction of Cu, Zn and Pb from natural water samples(Wiley Online Library, 2020-03-11) Aydın, Funda; Çakmak, Reşit; Levent, Abdulkadir; Soylak, MustafaA novel silica sorbent, silica gel‐immobilized 5‐aminoisophthalohydrazide (SiO2‐APH), was prepared by the condensation of 3‐chloropropyl‐functionalized silica gel with 5‐aminoisophthalohydrazide (APH) derived from dimethyl 5‐aminoisophthalate as a starting material and used for separation and preconcentration of Cu, Zn, and Pb metals in water samples using Flame Atomic Absorption Spectrometry (FAAS). The characterization of the new sorbent was carried out by Elemental Analysis, Thermogravimetric Analysis (TGA) and Fourier Transform Infrared Spectroscopy (FTIR). Important analytical parameters including as pH, amount of sorbent, type and amount of eluting solvent, sample volume, vortex and ultrasonic bath time, matrix ions that effect the developed SiO2‐APH‐solid phase extraction (SPE) method were investigated and optimum parameters were detected. Recoveries of examined metals were obtained as 98% for Cu and Pb and 101% for Zn. The relative standard deviation (RSD, n = 8) of Cu, Zn and Pb metals were 3.2, 2.8 and 1.6%, respectively. Limit of detections (LODs) (n = 10) were found as 2.7 μg L−1 for Cu, 7.4 μg L−1 for Zn and 3.5 μg L−1 for Pb μg L−1. The accuracy of the new method was assessed by analyzing of TMDA‐51.4 and TMDA‐70.2 certified reference materials. The results obtained for metals were in a good agreement with certified values. Addition/recovery test was applied to the real well, river, dam and stream water samples to check the accuracy of the method. The results showed that the developed SiO2‐APH‐SPE method can be effectively used as an alternative method for determination of Cu, Zn, and Pb metals in water samples.Öğe Synthesis and anticorrosion studies of 4-[(2-nitroacetophenonylidene)-amino]-antipyrine on SAE 1012 carbon steel in 15 wt.% HCl solution(Taylor & Francis, 2020-11-16) Gerengi, Hüsnü; Çakmak, Reşit; Dağ, Beşir; Solomon, M. M; Tüysüz Akbal, Hatice Aslıhan; Kaya, ErtuğrulA novel corrosion inhibitor, ((E)-1,5-dimethyl-4-((1-(3-nitrophenyl)ethylidene)amino)-2-phenyl-1,2-dihydro-3H-pyrazol-3-one) (DNPP) was synthesized in high yield by the condensation reaction of 4-aminoantipyrine with 2-nitroacetphenone derived from acetophenone as a starting material and characterized by FT-IR, 1H, and 13C NMR techniques. DNPP was tested against the corrosion of SAE 1012 carbon steel in 15 wt.% HCl solution using electrochemical and surface characterization techniques. Results obtained show that DNPP is effective in retarding the corrosion of SAE 1012 carbon steel. With 4 mM of DNPP, the charge transfer resistance of SAE 1012 in 15 wt.% HCl solution is raised from 17.42 to 140.50 Ω cm2 and the substrate surface is protected by 87%. The inhibition is through adsorption mechanism (mixed-adsorption type) and has been confirmed by SEM and EDAX results. Potentiodynamic polarization results reveal that DNPP acted as a mixed-type corrosion inhibitor. DNPP is a promising candidate for the formulation of an inhibitor cocktail for the strong acid environment.
