Application of time domain nuclear magnetic resonance (TD-NMR) for study of the distillation curve of petroleum

Crude oil distillates are a highly useful industrial product, mainly for energy generation. Unfortunately, they are rarely studied, mainly due to the low accessibility to products directly obtained from the distillation process, which is a laborious, expensive, and time-consuming operation. This work presents and discusses the use of time-domain nuclear magnetic resonance (TD-NMR) as a simple, affordable, and straightforward tool for the development of correlations supported on the transverse relaxation time (T₂) and boiling temperature. The results point out a high convergence between TD-NMR experimental data and the ASTM D2892 method for distillates from light, medium, and heavy oils, with up to 52.20% of accumulated mass and boiling point temperature (T_b) up to 400°C. Furthermore, an unprecedented relationship between T₂ values and the accumulated mass of the distillates is first demonstrated. This new insight opens new perspectives for future prediction of accumulated mass for unknown crude oils, placing the TD-NMR relaxometry as an appeal spectroscopy approach with a potential to meaningfully contribute to the daily refining petrochemical industry field operations.     

Simple and rapid determination of clonidine in pharmaceutical samples by voltammetry using a bare glassy carbon electrode

This work presents, for the first time, the voltammetric behavior of clonidine (CLO) drug and its determination, using an unmodified glassy carbon electrode (GCE). CLO exhibited only an irreversible oxidation process on the GCE, with peak potential at +0.85 V in pH 12 (vs Ag/AgCl). CLO oxidation process is pH-dependent and the electrochemical mechanisms on the GCE were proposed in acidic and basic medium. The determination of CLO was optimized in 0.1 mol L⁻¹ phosphate buffer solution at pH 12.0 using differential pulse voltammetry (DPV), which provides a good linear range (0.65 to 106.00 μmol L⁻¹) and low theoretical limit of detection (0.14 μmol L⁻¹) for the quality control of this drug in pharmaceutical samples. In addition, stable responses of CLO at the GCE were obtained in the same day (RSD = 3.4 %; n = 5) and different days (RSD = 2.0 %; n = 3). Moreover, the determination of CLO in a pharmaceutical formulation using the proposed GCE-DPV method presented good accuracy, since the recovery was close to 100 % and the dosing result was in agreement with an official method (HPLC-UV). The proposed method demonstrates a good analytical performance for CLO determination in pharmaceutical samples, providing a faster, simpler and lower-cost alternative for quality control of CLO than other reported methods.     

β-Cyclodextrin PAMAM Dendrimer Surface Doped with Silver and Hexacyanoferrate (III) and its Applications for Dopamine Detection in Synthetic Samples

A synthesis of β-cyclodextrin (β-Cd) functionalized with polyamide dendrimer PAMAM G.0 complexed with silver and potassium hexacyanoferrate (III) forming a mixed-valence complex (β-Cd-PAMAM-Ag/Fe) was proposed. This material was characterized by scanning electron microscopy (SEM), infrared spectroscopy (FT-IR), X-Ray diffraction (XRD), Energy Dispersion Spectroscopy (EDS) and Electron Paramagnetic Resonance (EPR). The hybrid complex was electrochemically investigated using cyclic voltammetry and some parameters (electrolyte, concentration of electrolyte, pH and scan rate) were evaluate in order to obtain optimum analytical responses. The β-Cd-PAMAM-Ag/Fe material was successfully applied in the electrocatalytic oxidation of dopamine (DOP) using Cyclic Voltammetry (CV) and Square Wave Voltammetry (SWV).