Fabrication of a sol–gel derived microporous zirconia membrane for nanofiltration

This paper reports the fabrication and nanofiltration properties of a sol–gel derived microporous zirconia membrane. Effects of synthesis parameters, including hydrolysis time, hydrolysis temperature, hydrolysis ratio and chelating agent dopant, on the state and size of polymeric zirconia sol, were investigated. Highly reproducible and stable zirconia sol after refluxing at 40 °C for 180 min, with an average particle size of approximately 8.6 nm, was synthesized with a recipe of [Zirconium n-propoxide]: [Diethanolamine]: [1-propanol]: [H₂O] being 1: 2.2: 28.7: 9.4 (in molar ratio). The sol was subsequently used for the fabrication of microporous ZrO₂ membranes onto alumina supported mesoporous γ-Al₂O₃ layers. ZrO₂ membranes with molecular weight cut-off (MWCO) of 354, 1,195, corresponding to the pore size of 0.94 and 1.75 nm, were successfully fabricated. Ionic retention properties of such ZrO₂ membranes with respect to electrolyte solutions, like MgCl₂, CaCl₂, NaCl and Na₂SO₄, were also determined. Effects of parameters such as concentration of salt solutions and trans-membrane pressure on retention rates of microporous ZrO₂ membranes were studied in detail. Results showed that zirconium n-propoxide derived microporous ZrO₂ membranes exhibited comparatively high retention rates towards divalent ions like Mg²⁺ and Ca²⁺, while much lower retention rates were observed for mono-valent ion (Na⁺) in the present study, which are the characteristics of nanofiltration membranes.     

Optimization of Pretreatment Method for Alkylmercuries Speciation in Coal by High‐Performance Liquid Chromatography Coupled with UV‐Digestion Cold Vapor Atomic Fluorescence Spectrometry

Abstract

Exhaustive extraction of analytes in their original chemical forms from samples with complex matrices is a pivotal step for speciation analysis. Herein we propose a pretreatment method for extracting and preconcentrating methylmercury and ethylmercury from coal samples by using KBr–H₂SO₄/CuSO₄–C₆H₅CH₃–Na₂S₂O₃ system. The extraction conditions, including the volume of the organic phase and the extraction time, were optimized in detail. Speciation analysis of alkylmercuries was carried out by high‐performance liquid chromatography online coupled with UV‐digestion and cold vapor atomic fluorescence spectrometry. The detection limits were 0.6 ng mL^?1 for methylmercury and 1 ng mL^?1 for ethylmercury, respectively. The recoveries of methylmercury and ethylmercury spiked in a sample were 84% and 82%, respectively. The method was applied successfully to analysis of alkylmercuries in four coal samples collected from northeast China.     

Tuner design and RF test of a four-rod RFQ

A mini-vane four-rod radio frequency quadruple (RFQ) accelerator has been built for neutron imaging. The RFQ will operate at 201.5 MHz, and its length is 2.7 m. The original electric field distribution along the electrodes is not flat. The resonant frequency needs to be tuned to the operating value. And the frequency needs to be compensated for temperature change during high power RF test and beam test. As tuning such a RFQ is difficult, plate tuners and stick tuners are designed. This paper will present the tuners design, the tuning procedure, and the RF properties of the RFQ.

     

Development and validation of UPLC‐MS/MS method for determination of domperidone in human plasma and its pharmacokinetic application

A sensitive, rapid and selective ultra‐performance liquid chromatography–tandem mass spectrometric (UPLC‐MS/MS) method was developed for the determination and pharmacokinetic study of domperidone in human plasma. Diphenhydramine was used as the internal standard. Plasma sample pretreatment involved a one‐step liquid–liquid extraction with a mixture of diethyl ether–dichloromethane (3:2, v/v). The analysis was carried out on an Acquity UPLC^TM BEH C₁₈ column. The mobile phase consisted of methanol–water containing 10 mmol/L ammonium acetate and 0.5% (v/v) formic acid (60:40, v/v). The detection was performed on a triple quadrupole tandem mass spectrometer in multiple reaction monitoring mode via electrospray ionizationsource with positive mode. Each plasma sample was chromatographed within 2.1 min. The standard curves for domperidone were linear (r² ≥ 0.99) over the concentration range of 0.030–31.5 ng/mL with a lower limit of quantification of 0.030 ng/mL. The intra‐ and inter‐day precision (relative standard deviation) values were not higher than 13% and accuracy (relative error) was from ?7.6 to 1.2% at three quality control levels. The method herein described was superior to previous methods and was successfully applied to the pharmacokinetic study of domperidone in healthy Chinese volunteers after oral administration. Copyright © 2012 John Wiley & Sons, Ltd.