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Öğe Synthesis, characterization and application of a novel multifunctional stationary phase for hydrophilic interaction/reversed phase mixed-mode chromatography(Talanta, 2017-11-1) Aral, Tarık; Aral, Hayriye; Çelik, Kadir Serdar; Altındağ, RamazanA novel multifunctional stationary phase based on silica gel was synthesised starting from L- isoleucine and 4-phenylbutylamine and evaluated as a hydrophilic interaction/reversed-phase mixed-mode stationary phase for high-performance liquid chromatography (HPLC). The prepared stationary phase was characterized by elemental analysis, infrared spectroscopy (IR), scanning electron microscopy (SEM), Brunauer, Emmett and Teller (BET) and solid-state 13C nuclear magnetic resonance (NMR). The mechanisms involved in the chromatographic separation are multi-interaction, including hydrophobic, π-π, hydrogen-bonding, dipole-dipole and ion-dipole interactions. Based on these interactions, successful separation could be achieved among several aromatic compounds having different polarities under both hydrophilic interaction liquid chromatography (HILIC) and reversed phase (RP) condition. Nucleotides/nucleosides were separated in the HILIC mode. The effects of different separation conditions, such as pH value, mobile-phase content, column temperature, buffer concentration and flow rate, on the separation of nucleotides/nucleosides in HILIC mode were investigated. The seven nucleotides/nucleosides were separated within 22 min, while six of them were separated within 10 min by isocratic elution. To determine the influence of the new multifunctional stationary phase under the RP condition, a number of moderately and weakly polar and nonpolar compounds, such as 10 substituted anilines and eight substituted phenols were separated successfully under the RP condition within 14 and 15 min, respectively. Additionally, nine mixtures of polar/nonpolar test compounds were simultaneously separated within 19 min, while seven of them were separated within 12 min, under HILIC/RP mixed-mode conditions. Chromatographic parameters, such as the retention factor and peak asymmetry factor, were calculated for all of the analytes, while the theoretical plate number was calculated for analytes separated by isocratic elution. Compared to traditional C18 and commercial HILIC columns, the new stationary phase exhibited both HILIC and RPLC performance, and the scope of analyte separation was thus enlarged.Öğe I-V-T analysing an inhomogeneous Au/Poly(4-vinyl phenol)/p-Si structure with a double gaussian distribution of barrier heights(Springer Nature, 2010-12-29) Pakma, Osman; Tozlu, Cem; Kavasoğlu, Neşe; Kavasoğlu, Abdülkadir Sertap; Özden, ŞadanIn this study, the current-voltage (I-V) characteristics of Au/Poly(4-vinyl phenol)/p-Si structures have been measured over a wide temperature range (100-300 K). These structures have been analyzed according to thermionic emission (TE) theory, as a result of which an abnormal decrease occurred in the zero-bias barrier height (φb0) and an increase in the ideality factor (n) was observed with temperature decrease and nonlinearity in the activation energy plot. By assuming a Gaussian distribution (GD) of barrier heights of the Au/Poly(4-vinyl phenol)/p-Si structures, barrier inhomogeneities are believed to responsible for this behavior. Evidence is given for the existence of a double GD with mean barrier heights (φ̄b0) of 1.042 and 0.623 eV, standard deviations of 0.138 and 0.081 V, and ideality factors 2.76 and 7.26, which remain effective in the temperature ranges of 180-300 and 100-160 K, respectively. As a result, without using the temperature coefficient of the barrier height, the modified ln(Io/T 2)-q2σo 2/2(kT)2 vs. q/kT plot gives φ̄b0 values and Richardson constants (A *) as 1.036 and 0.623 eV, and 36.20 and 19.99 A/cm2 K2, respectively. The effective Richardson constant value of 36.20 A/cm2 K2 is very similar to the theoretical value of 32 A/cm2K2 for p-Si. Consequently, the temperature dependence of the forward bias I-V characteristics of Au/Poly(4-vinyl phenol)//p-Si (MIS) structure could be attributed to the thermionic emission (TE) mechanism with double GD of the barrier heights.Öğe Sensitive voltammetric determination of testosterone in pharmaceuticals and human urine using a glassy carbon electrode in the presence of cationic surfactant(Elsevier, 2014-05-10) Levent, Abdulkadir; Altun, Ahmet; Yardım, Yavuz; Şentürk, ZühreIn this work, the electrochemical investigation of testosterone, a steroid hormone from the androgen group, was carried out in aqueous and aqueous/surfactant solutions using a glassy carbon (GC) electrode. In cyclic voltammetry, the compound showed one irreversible and adsorption-controlled reduction peak. Addition of cationic surfactant (cetyltrimethylammonium bromide, CTAB) was found to enhance the reduction current signal of testosterone, whereas, anionic (sodium dodecylsulfate, SDS) and non-ionic (Tween 80) surfactants exhibited opposite effect. Using square-wave adsorptive stripping voltammetry, the current showed a linear dependence with concentration in the range between 10 and 70 nM in Britton–Robinson buffer, pH 5.0 containing 3 mM CTAB. A detection limit of 1.18 nM (0.34 ng mL−1), and relative standard deviation of 4.12% for a concentration level of 35 nM (n = 11) were calculated. This method was successfully applied for the analysis of testosterone in oil-based pharmaceutical preparations and urine samples without any separation.Öğe Graphene/Nafion composite film modified glassy carbon electrode for simultaneous determination of paracetamol, aspirin and caffeine in pharmaceutical formulations(ScienceDirect, 2016-05-16) Yiğit, Aydın; Yardım, Yavuz; Çelebi, Metin; Levent, Abdulkadir; Şentürk, ZühreA graphene-Nafion compositefilm was fabricated on the glassy carbon electrode (GR-NF/GCE), and usedfor simultaneous determination of paracetamol (PAR), aspirin (ASA) and caffeine (CAF). The electro-chemical behaviors of PAR, ASA and CAF were investigated by cyclic voltammetry and square-waveadsorptive anodic stripping voltammetry. By using stripping one for simultaneous determination of PAR,ASA and CAF, their electrochemical oxidation peaks appeared atþ0.64, 1.04 and 1.44 V, and good linearcurrent responses were obtained with the detection limits of 18 ng mL 1(1.2 10 9M), 11.7 ng mL 1(6.5 10 8M) and 7.3 ng mL 1(3.8 10 8M), respectively. Finally, the proposed electrochemical sensorwas successfully applied for quantifying PAR, ASA and CAF in commercial tablet formulations.Öğe Voltammetric behavior of benzo[a]pyrene at boron-doped diamond electrode: A study of its determination by adsorptive transfer stripping voltammetry based on the enhancement effect of anionic surfactant, sodium dodecylsulfate(Elsevier, 2011-07-15) Yardım, Yavuz; Keskin, Ertuğrul; Levent, Abdulkadir; Şentürk, ZühreBenzo[a]pyrene (BaP), a member of the polycyclic aromatic hydrocarbon (PAH) class, is one of the most potent PAH carcinogens. The electrochemical oxidation of BaP was first studied by cyclic voltammetry at the boron-doped diamond electrode in non-aqueous solvent (dimethylsulphoxide with lithium perchlorate). The compound was irreversibly oxidized in a single step at high positive potential, resulting in the well-resolved formation of a couple with a reduction and re-oxidation wave at much lower potentials. Special attention was given to the use of adsorptive stripping voltammetry together with a medium exchange procedure in aqueous and aqueous/surfactant solutions over the pH range of 2.0–8.0. The technique in aqueous solutions had little value in practice because of too small oxidation peak current. This problem was solved when surfactants were added into the sample solution, by which the oxidation peak currents of BaP were found enhanced dramatically. The employed surfactants were sodium dodecylsulfate (anionic, SDS), cetyltrimethylammonium bromide (cationic, CTAB) and Tween 80 (non-ionic). Using square-wave stripping mode, the compound yielded a well-defined voltammetric response in Britton–Robinson buffer, pH 2.0 containing 2.5 × 10−4 M SDS at +1.07 V (vs. Ag/AgCl) (after 120 s accumulation at +0.10 V). The process could be used to determine BaP in the concentration range of 16–200 nM (4.04–50.46 ng mL−1), with a detection limit of 2.86 nM (0.72 ng mL−1). This method was also applied to determine BaP in model water sample prepared by adding its different concentrations into tap water.Öğe The analysis of the charge transport mechanism of n-Si/MEH-PPV device structure using forward bias I-V-T characteristics(Elsevier, 2010-03-04) Kavasoğlu, Abdülkadir Sertap; Yakuphanoğlu, Fahrettin; Kavasoğlu, Neşe; Pakma, Osman; Birgi, Özcan; Oktik, ŞenerIn this study, temperature dependent current-voltage (I-V) measurements and investigation of the dc current transport mechanism of n-Si/MEH-PPV device have been performed. While the series resistance value displayed strongly temperature dependent behaviour, the ideality factor varied between 3.2 and 1.8 in the temperature range 110-330 K. The temperature dependent ideality factor behaviour at low temperature region (110-220 K) shows that tunnelling enhanced recombination is valid rather than thermionic emission theory and the characteristic tunnelling energy is calculated as 30 meV. There is a slightly linear relationship between the ideality factor and temperature at region II (230-330 K) which is attributed to drift-diffusion current transport in the n-Si/MEH-PPV device as stated already by Osvald.
