Fabrication of a highly sensitive electrochemiluminescence lactate biosensor using ZnO nanoparticles decorated multiwalled carbon nanotubes

ZnO nanoparticles (nanoZnO) were decorated on multiwalled carbon nanotubes (MWCNTs) and then the prepared nano-hybrids, nanoZnO-MWCNTs, were immobilized on the surface of a glassy carbon electrode (GCE) to fabricate nanoZnO-MWCNTs modified GCE. The prepared electrode, GCE/nanoZnO-MWCNTs, showed excellent electrocatalytic activity towards luminol electrochemiluminescence (ECL) reaction. The electrode was then further modified with lactate oxidase and Nafion to fabricate a highly sensitive ECL lactate biosensor. Two linear dynamic ranges of 0.01-10 μmol L⁻¹ and 10-200 μmol L⁻¹ were obtained for lactate with the correlation coefficient better than 0.9996. The detection limit (S/N = 3) was 4 nmol L⁻¹ lactate. The relative standard deviation for repetitive measurements (n = 6) of 10 μmol L⁻¹ lactate was 1.5%. The fabrication reproducibility for five biosensors prepared and used in different days was 7.4%. The proposed ECL lactate biosensor was used for determination of lactate in human blood plasma samples with satisfactory results.     

Enhanced electrochemiluminescence from luminol at multi-walled carbon nanotubes decorated with palladium nanoparticles: a novel route for the fabrication of an oxygen sensor and a glucose biosensor

Incorporation of palladium nanoparticles on the surface of multi-walled carbon nanotubes and modification of glassy carbon electrode with the prepared nano-hybrid material led to the fabrication of a novel electrode. The modified electrode showed attractive electrocatalytic activity and sensitizing effect on luminol-O(2) and luminol-H(2)O(2) electrochemiluminescence (ECL) reactions at neutral media. The sensitized luminol-O(2) and luminol-H(2)O(2) reactions were successfully applied for the ECL determination of dissolved O(2) and glucose, respectively. Under the optimal conditions for luminol-O(2) system, the ECL signal intensity of luminol was linear with the concentration of dissolved oxygen in the range between 0.08 and 0.94 mM (r=0.9996) and for luminol-H(2)O(2) system, the ECL signal intensity of luminol was linear with the concentration of glucose in the range between 0.1 and 1000 μM (r=0.9998). The limits of detection (S/N=3) for dissolved oxygen and glucose were 0.02 mM and 54 nM, respectively. The relative standard deviations (RSD) for repetitive measurements of 0.50 mM oxygen (n=10) and 10 μM glucose (n=30) were 3.5% and 0.3%, respectively. Also, under the optimal conditions for luminol-H(2)O(2) system, the ECL signal intensity of luminol was linear with the concentration of H(2)O(2) in the range between 1 nM and 0.45 mM (r=0.9997). The limit of detection (S/N=3) for H(2)O(2) detection was 0.5 nM and the relative standard deviation for repetitive measurements of 10 μM H(2)O(2) (n=10) was 0.8%.     

Elemental compositions from daughter ion spectra of m1+ and [m1 + 1]+: Some applications of the method

The elemental compositions of ions can be determined in tandem mass spectrometry by comparing the daughter ion spectra of the m₁⁺ and [m₁ + 1]⁺ ions. The method is demonstrated for mass-analyzed ion kinetic energy spectra but is applicable to all types of daughter ion spectra, including complex collisionally activated dissociation spectra. In this work, the method is applied to compounds that produce daughter ions of known elemental compositions, and the errors and limitations are evaluated. Following that test, the procedure is applied to a compound that may produce daughters of more than one possible elemental composition. The method is sometimes useful even if the formula of the parent is not known; that is, the formulae of unknown parent and daughter ions may be found. Locating a specific atom in an isotopically labeled molecule is another capability of the method. The basic equation of the method was generalized and incorporated into a computer program for performing the calculations.     

Ionic Liquid Based Ultrasound-Assisted Emulsification Microextraction for Preconcentration of Phenol Using Central Composite Design

In this work, phenol reacted with 4-aminoantipyrine (4-AAP) reagent in presence of potassium hexacyanoferrate(III) and then was extracted using ultrasound-assisted emulsification microextraction via 1-hexyl-3-methyl imidazolium hexafluorophosphate as an environmentally friendly solvent. Effects of the main experimental variables were investigated and optimized by central composite design. Under the optimum conditions (pH 9.5, 100 mg/L 4-AAP, 100 μL of ionic liquid as extraction solvent, 0.2 g/L K₃Fe(CN)₆ and 0.2 M NH₄Cl) the dynamic linear range, limit of detection and relative standard deviation were obtained as 0.2?25 μg/L, 0.07 μg/L and 2.6%, respectively. Finally, the applicability of the proposed ultrasoundassisted emulsification microextraction was examined and very good results were obtained. The results confirmed the applicability of the proposed method as a versatile, low cost and sensitive preconcentration method for determination of very low concentrations of phenol in aqueous solutions.     

Micelle-mediated extraction for simultaneous spectrophotometric determination of aluminum and beryllium using mean centering of ratio spectra

A new micelle-mediated extraction method for preconcentration of ultra-trace quantities of beryllium and aluminum as a prior step to their simultaneous spectrophotometric determination has been developed. Chrome Azurol S (CAS), cetyltrimethylammonium bromide (CTAB) and Triton X-114 were used as chelating agent, cationic surfactant for extraction and co-extraction agent, respectively. Mean centering (MC) of ratio spectra has been used for simultaneous analysis of beryllium and aluminum. The optimal extraction and reaction conditions were studied, and the analytical characteristics of the method (e.g., limit of detection, linear range, preconcentration, and improvement factors) were obtained. Linearity was obeyed in the range of 5-40 ng mL⁻¹ of beryllium and 3-100 ng mL⁻¹ of aluminum. The detection limit of the method is 0.98 and 0.52 ng mL⁻¹ for beryllium and aluminum, respectively. The interference effect of some anions and cations was also tested. The method was applied to the simultaneous determination of beryllium in water samples.     

Catalytic reactions of chlorofluoroethanes at fluorinated alumina and chromia aerogels and xerogels: A comparison of reaction pathways in alumina- and chromia-based catalysts

The differences in the dynamic behaviour of 1,1,2-trichlorotrifluoroethane over fluorinated alumina or chromia catalysts at moderate temperatures are significant. Alumina-based catalysts favour the isomerization of CCl₂FCClF₂ followed by the dismutation of CCl₃CF₃ so formed. Fluorinated chromias are less selective since halogen exchange and isomerization reactions both occur. An explanation in terms of the differences in Al---X, X=Cl or F, bond energies compared with their Cr---X counterparts is suggested. The identity of the catalyst precursor has little effect in the chromium case and no effect in the case of aluminium.     

Determination of trace elements in tea leaves by neutron activation analysis

Instrumental neutron activation analysis has been employed to determine 14 trace elements in two brands of Iranian and foreign tea. The elements are: Br, La, Ba, K, Mn, Cl, Cr, Cs, Rb, Fe, Co, Zn, Sc and Au. The transference ratio of the elements into solution, when tea is leached by percolation, is also reported. It was found that some elements are totally transferred into solution and some are partially retained by the leaves.     

Adsorption isotherms and ideal selectivities of hydrogen sulfide and carbon dioxide over methane for the Si-CHA zeolite: comparison of carbon dioxide and methane adsorption with the all-silica DD3R zeolite

Adsorption isotherms of H₂S, CO₂, and CH₄ on the Si-CHA zeolite were measured over pressure range of 0–190 kPa and temperatures of 298, 323, and 348 K. Acid gases adsorption isotherms on this type of zeolite are reported for the first time. The isotherms follow a typical Type-I shape according to the Brunauer classification. Both Langmuir and Toth isotherms describe well the adsorption isotherms of methane and acid gases over the experimental conditions tested. At room temperature and pressure of 100 kPa, the amount of CO₂ adsorption for Si-CHA zeolite is 29 % greater than that reported elsewhere (van den Bergh et al. J Mem Sci 316:35–45 (2008); Surf Sci Catal 170:1021–1027 (2007)) for the pure silica DD3R zeolite while the amounts of CH₄ adsorption are reasonably the same. Si-CHA zeolite showed high ideal selectivities for acid gases over methane at 100 kPa (6.15 for H₂S and 4.06 for CO₂ at 298 K). Furthermore, H₂S adsorption mechanism was found to be physical, and hence, Si-CHA can be utilized in pressure swing adsorption processes. Due to higher amount of carbon dioxide adsorbed and lower heats of adsorption as well as three dimensional channels of Si-CHA pore structure, this zeolite can remove acid gases from methane in a kinetic based process such as zeolite membrane.     

Dispersive liquid-liquid microextraction of Fe(II) and Cu(II) with diethyldithiocarbamate and their simultaneous spectrophotometric determination using mean centering of ratio spectra

A new dispersive liquid-liquid microextraction (DLLME) method for preconcentration of trace quantities of Fe(II) and Cu(II) followed by their spectrophotometric determination has been developed. For the extraction, an appropriate mixture of ethanol (the disperser solvent) and carbon tetrachloride (the extraction solvent) was injected rapidly into the water sample containing Fe(II) and Cu(II) after formation of complexes with diethyldithiocarbamate. Mean centering (MC) of ratio spectra has been used for simultaneous determination of Fe(II) and Cu(II). Linear range of the method is 1.0–100 ng/mL for Fe(II) and 0.3–100 ng/mL for Cu(II), the detection limit is 0.53 ng/mL and 0.14 ng/mL Cu(II), resp. The interference effect of some anions and cations is reported. The method was applied to the determination of Fe(II) and Cu(II) in well water samples.     

Interference peaks in mass analysed ion kinetic energy spectra

When mass analysed ion kinetic energy spectroscopy is performed on ions of low abundance and low mass compared with the rest of the ions present in the ion chamber, severe interference may be observed. The major form taken by the interference is of narrow peaks at non-integral mass numbers. Many such peaks can be observed in mass analysed ion kinetic energy spectra and they are mainly attributed to decompositions of metastable ions occurring in the first field free region of the reversed geometry double focusing mass spectrometer.