Magnetic Fe-SBA-15 mesoporous silica molecular sieves were prepared, characterized, and used for magnetic separation. Wet impregnation, drying, and calcination steps led to iron inclusion within the mesopores. Iron oxide was reduced to the metal form with hydrogen, and the magnetic Fe-SBA-15 was obtained. Fourier-transform infrared spectroscopy confirmed the preparation process from the oxide to metal forms. The structure of magnetic materials was confirmed by Mössbauer spectra. Powder X-ray diffraction data indicated that the structure of Fe-SBA-15 retained the host SBA-15 structure. Brunauer-Emmett-Teller analysis revealed a decrease in surface area and pore size, indicating Fe-SBA-15 coating on the inner surfaces. Scanning electron micrographs confirmed the decrease in size for modified SBA-15 particles. From scanning electron micrographs, it was found that the size of the modified SBA-15 particles decreased. Transmission electron micrographs also confirmed that modified SBA-15 retained the structure of the parent SBA-15 silica. Fe-SBA-15 exhibited strong magnetic properties, with a magnetization value of 8.8 emu g<sup>-1</sup>. The iron content in Fe-SBA-15 was determined by atom adsorption spectroscopy. Fe-SBA-15 was successfully used for the magnetic separation of three aromatic compounds in water. Our results suggest wide applicability of Fe-SBA-15 magnetic materials for the rapid and efficient separation of various compounds.

Huayu Huang

Yongsheng Ji

Zhenfeng Qiao

Chuande Zhao

Jianguo He

Haixia Zhang

Preparation, Characterization, and Application of Magnetic Fe-SBA-15 Mesoporous Silica Molecular Sieves

A new flow procedure based on multicommutation with chemiluminometric detection was developed to quantify gentamicin sulphate in pharmaceutical formulations. This approach is based on gentamicin's ability to inhibit the chemiluminometric reaction between luminol and hypochlorite in alkaline medium, causing a decrease in the analytical signal. The inhibition of the analytical signal is proportional to the concentration of gentamicin sulphate, within a linear range of 1 to 4&#x2009;<svg style="vertical-align:-2.29482pt;width:9.6374998px;" id="M1" height="9.6750002" version="1.1" viewBox="0 0 9.6374998 9.6750002" width="9.6374998"  xmlns="http://www.w3.org/2000/svg">
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</svg>g&#x2009;mL<sup  >-1</sup> with a coefficient variation  &#x3c;3&#x25;. A sample throughput of 55 samples h<sup  >-1</sup> was obtained. The developed method is sensitive, simple, with low reagent consumption, reproducible, and inexpensive, and when applied to the analysis of pharmaceutical formulations (eye drops and injections) it gave results with RSD between 1.10 and 4.40&#x25;.

Lúcia H. M. L. M. Santos

A. N. Araújo

Boaventura Reis

M. C. B. S. M. Montenegro

Development of a Multicommutated Flow System with Chemiluminometric Detection for Quantification of Gentamicin in Pharmaceuticals

The present research is focused on automation, miniaturization, and system interaction with high throughput for multiple and specific Direct Immersion-Solid Phase Microextraction/Fast Gas Chromatography analysis of the urinary ketones. The specific Mass Spectrometry instrumentation, capable of supporting such the automated changeover from Negative Chemical to Electron Ionization mode, as well as the automation of the preparation procedure by new device called MultiFiber Exchange, through change of the fibers, allowed a friendly use of mass spectrometry apparatus with a number of advantages including reduced analyst time and greater reproducibility (2.01&#x2013;5.32&#x25;). The detection limits for the seven ketones were less than 0.004&#x2009;mg/L. For an innovative powerful meaning in high-throughput routine, the generality of the structurally informative Mass Spectrometry fragmentation patterns together with the chromatographic separation and software automation are also investigated.

Marco Pacenti

Stefano Dugheri

Pietro Traldi

Filippo Degli Esposti

Nicola Perchiazzi

Elena Franchi

Massimo Calamante

Ireneo Kikic

Paolo Alessi

Alice Bonacchi

Edoardo Salvadori

Giulio Arcangeli

Vincenzo Cupelli

New Automated and High-Throughput Quantitative Analysis of Urinary Ketones by Multifiber Exchange-Solid Phase Microextraction Coupled to Fast Gas Chromatography/Negative Chemical-Electron Ionization/Mass Spectrometry

A simple, rapid and sensitive method was proposed for online determination of tannic acid in colored tannery wastewater by automatic reference flow injection analysis. Based on the tannic acid reduction phosphotungstic acid to form blue compound in pH 12.38 alkaline solutions, the shade of blue compound is in a linear relation to the content of tannic acid at the point of the maximum absorption peak of 760&#x2009;nm. The optimal experimental conditions had been obtained. The linear range of the proposed method was between 200&#x2009;<svg style="vertical-align:-2.29482pt;width:9.6374998px;" id="M1" height="9.6750002" version="1.1" viewBox="0 0 9.6374998 9.6750002" width="9.6374998"  xmlns="http://www.w3.org/2000/svg">
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</svg> to 80&#x2009;mg <svg style="vertical-align:-0.0pt;width:23.262501px;" id="M3" height="13.775" version="1.1" viewBox="0 0 23.262501 13.775" width="23.262501"  xmlns="http://www.w3.org/2000/svg">
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</svg> and the detection limit was 0.58&#x2009;<svg style="vertical-align:-2.29482pt;width:9.6374998px;" id="M4" height="9.6750002" version="1.1" viewBox="0 0 9.6374998 9.6750002" width="9.6374998"  xmlns="http://www.w3.org/2000/svg">
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</svg>. The relative standard deviation was 3.08&#x25; and 2.43&#x25; for 500&#x2009;<svg style="vertical-align:-2.29482pt;width:9.6374998px;" id="M6" height="9.6750002" version="1.1" viewBox="0 0 9.6374998 9.6750002" width="9.6374998"  xmlns="http://www.w3.org/2000/svg">
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</svg> of tannic acid standard solution, respectively, (<svg style="vertical-align:-0.17555pt;width:42.912498px;" id="M9" height="10.9125" version="1.1" viewBox="0 0 42.912498 10.9125" width="42.912498"  xmlns="http://www.w3.org/2000/svg">
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</svg>). The method had been successfully applied to determination of tannic acid in colored tannery wastewaters and the analytical results were satisfactory.

Liang Wei

Online Determination of Trace Amounts of Tannic Acid in Colored Tannery Wastewaters by Automatic Reference Flow Injection Analysis

A new method was developed for simultaneous determination of copper, lead, and cadmium, based on their voltammetric response at a carbon paste electrode modified with hexagonal mesoporous silica (HMS) immobilized quercetin (HMS-Qu/CPE). Compared with quercetin modified carbon paste electrode (Qu/CPE) and quercetin ionic liquid modified carbon paste electrode (Qu-IL/CPE), the HMS-Qu/CPE exhibited improved selectivity and high sensitivity toward the detection of copper, lead, and cadmium. The properties of the HMS-Qu/CPE in 0.1 M HCOONa-HCl buffer solution (pH4.7) were investigated by adsorptive stripping voltammetry (ASV) and electrochemical impedance spectroscopy (EIS). The electrochemical behavior of copper, lead, and cadmium at the modified electrodes and factors affecting the preconcentration procedures were also investigated. Detection limits of 5.0, 0.8, 1.0 nM for copper, lead, and cadmium were obtained, respectively. The method is simple, fast, sensitive, and selective, and is successfully applied to soil sample.

Fangquan Xia

Xin Zhang

Changli Zhou

Danzi Sun

Yanmin Dong

Zhen Liu

Simultaneous Determination of Copper, Lead, and Cadmium at Hexagonal Mesoporous Silica Immobilized Quercetin Modified Carbon Paste Electrode

A fully automated and fast pneumatic transport system for short-time activation analysis was recently developed. It is suitable for small nuclear research reactors or laboratories that are using neutron generators and other neutron sources. It is equipped with a programmable logic controller, software package, and 12 devices to facilitate optimal analytical procedures. 550&#x2009;ms were only necessary to transfer the irradiated capsule (diameter: 15&#x2009;mm, length: 50&#x2009;mm, weight: 4 gram) to the counting chamber at a distance of 20 meters using pressurized air (4 bars) as a transport gas.

S. S. Ismail

A New Automated Sample Transfer System for Instrumental Neutron Activation Analysis

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<p><em>Journal of Analytical Methods in Chemistry</em> publishes research into the methods and instrumentation used in chemical analysis, including spectroscopic, spectrometric and wet chemistry techniques, and their applications in real-world problems.</p>


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<p>Chief Editor, Dr. María José Trujillo-Rodríguez, is based in the Chemistry Department (Analytical Chemistry Division) at Universidad de La Laguna, Spain.</p>


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Journal of Analytical Methods in Chemistry publishes research into the methods and instrumentation used in chemical analysis, including spectroscopic, spectrometric and wet chemistry techniques, and their applications in real-world problems.

Journal of Analytical Methods in Chemistry