RESUMO
An electroanalytical sensor was constructed constituted on a carbon paste electrode (CPE) with a ZIF-67 modifier and devoted to the quantification of Tl(I). Several characterization tests including XRD, BET, FT-IR, SEM/EDS/mapping, TEM, impedance spectroscopy (EIS), and cyclic voltammetry (CV) were performed on the synthesized ZIF-67 nanocrystals and CPE matrix. Central composite design (CCD) was used to assess the impact of variables affecting the sensor response, including the weight percent of ZIF-67 (14%), the pH of the thallium accumulation solution (6.4), and accumulation time (315 s) as well as the accumulation potential (-1.2 V). The direct linear relationship between the sensor response and the concentration of Tl(I) is in the interval of 1.0×10-10 to 5.0×10-7 M (coefficient of determination = 0.9994). The detection limit is approximately 1.0 × 10-11 M. The right selection of the MOF makes this sensor highly resistant to the interference of other ions. High selectivity against common interferences in the measurement of thallium (such as Pb(II) and Cd(II)) is an important feature of this sensor. To confirm the performance of the prepared sensor, the amount of thallium in the real sample was determined.
RESUMO
ZIF-8 was synthesized and carbon paste electrodes (CPEs) modified with this metal-organic framework were utilized for quantitation of silver(i) by the differential pulse anodic stripping voltammetry (DPASV) technique.Prepared ZIF-8 and the matrix of the electrodes were distinguished by impedance spectroscopy (EIS), XRD, FT-IR spectroscopy, cyclic voltammetry (CV), TEM and SEM/EDX methods. To obtain the strongest stripping peak currents, several significant variables were optimized with response surface methodology (RSM), including the ligand amount (near 11% w/w), applied potential for preconcentration (approximately -1.36 V), pH of the preconcentration solution (about 8.5) and preconcentration time (about 275 s). A calibration curve was acquired in the limits from 1.0 × 10-10 to 5.0 × 10-7 M with the Pearson correlation coefficient R = 0.9993. The limiting detectable concentration (LDC) was determined to be 1.0 × 10-11 M. The developed sensor has high selectivity for mercury(ii). The excellent pH, potential and especially size-exclusion based selectivity of the prepared sensor are unique characteristics that are very important in the determination of silver ions. The developed method was effectively employed for the quantitation of silver(i) ions in environmental and industrial samples.
RESUMO
A nitrogen center was abstracted from a pyrrolyl ring to form the dinuclear nitrido- and dienyl-bridged complex 1 during the reaction of [{(tmeda)NbII Cl}2 (µ-Cl)3 Li(tmeda)] with the lithium salt of 2,5-dimethylpyrrole (tmeda=N,N,N',N'-tetramethylethylenediamine). A second product from this reaction is the amido-carbene-hydride niobium complex 2, which likewise forms under C-N bond cleavage.
