Capillary electrophoresis on-line coupled with hydride generation-atomic fluorescence spectrometry for speciation analysis of selenium

A new method for speciation analysis of two inorganic selenium species was developed by on-line coupling of capillary electrophoresis (CE) with hydride generation-atomic fluorescence spectrometry (HG-AFS) and on-line conversion of Se(VI) to Se(IV). Baseline separation of Se(VI) and Se(IV) was achieved by CE in a 50 cm x 75 microm inside diameter (ID) fused-silica capillary at -20 kV using a mixture of 15 mmol.L(-1) NaH2PO4 and 0.5 mmol.L(-1) cetyltrimethylammonium bromide (pH 7.5) as electrolyte buffer. Se(VI) was on-line reduced to Se(IV) by mixing the CE effluent with concentrated HCl. The precision (relative standard deviation, RSD, n=7) ranged from 0.7 to 1.3% for migration time, 6.4 to 3.7% for peak height response, and 5.9 to 6.1% for peak area for the two selenium species at the 500 microg.L(-1) (as Se) level. The detection limits were 33 and 25 microg.L(-1) (as Se) for Se(VI) and Se(IV), respectively. The recoveries of the two selenium species in five locally collected water samples ranged from 88 to 114%. The developed method was applied to speciation analysis of inorganic selenium species in spiked natural water samples.     

Determination of gadolinium-based MRI contrast agents in biological and environmental samples: A review

The development of analytical methods and strategies to determine gadolinium and its complexes in biological and environmental matrices is evaluated in this review.     

Differentiation and characterization of isotopically modified silver nanoparticles in aqueous media using asymmetric-flow field flow fractionation coupled to optical detection and mass spectrometry

The principal objective of this work was to develop and demonstrate a new methodology for silver nanoparticle (AgNP) detection and characterization based on asymmetric-flow field flow fractionation (A4F) coupled on-line to multiple detectors and using stable isotopes of Ag. This analytical approach opens the door to address many relevant scientific challenges concerning the transport and fate of nanomaterials in natural systems. We show that A4F must be optimized in order to effectively fractionate AgNPs and larger colloidal Ag particles. With the optimized method one can accurately determine the size, stability and optical properties of AgNPs and their agglomerates under variable conditions. In this investigation, we couple A4F to optical absorbance (UV–vis spectrometer) and scattering detectors (static and dynamic) and to an inductively coupled plasma mass spectrometer. With this combination of detection modes it is possible to determine the mass isotopic signature of AgNPs as a function of their size and optical properties, providing specificity necessary for tracing and differentiating labeled AgNPs from their naturally occurring or anthropogenic analogs. The methodology was then applied to standard estuarine sediment by doping the suspension with a known quantity of isotopically enriched ¹⁰⁹AgNPs stabilized by natural organic matter (standard humic and fulvic acids). The mass signature of the isotopically enriched AgNPs was recorded as a function of the measured particle size. We observed that AgNPs interact with different particulate components of the sediment, and also self-associate to form agglomerates in this model estuarine system. This work should have substantial ramifications for research concerning the environmental and biological fate of AgNPs.     

空空导弹测试系统应用LXI总线研究

首先对空空导弹测试系统应用各种仪器总线的情况进行了分析研究,然后介绍了一台PXI总线测试设备的改造方案,该方案中设计了一套基于LXI总线控制的电源子系统,该子系统与PXI主系统一起形成了新的混合总线控制测试设备。该改造方案实现了改造需求中的低成本和小型化设计。同时,结合该方案分析了LXI总线在空空导弹测试系统上应用的优缺点和现阶段局限性。提出了空空导弹测试系统应向着通用、开放和网络化方向发展的观点,得出了未来的空空导弹测试系统将是包含GPIB、VXI、PXI、LXI等总线接口的合成系统,各总线接口仅是网络上的一个节点的结论。     

KBA显微镜成像系统的成像模拟及X光成像实验的研究

KBA显微镜是一种非轴对称、非共轴的掠入射成像系统。其结构复杂,调节精度要求很高,在实际成像实验操作中难以掌握其成像特性。利用光学设计软件模拟其成像,对系统的调节和成像分析提供有益的参考。利用光学设计软件ZEMAX模拟了KBA显微镜对点源的成像过程,给出了KBA显微镜成像系统的焦深约为1 mm,景深为50 mm左右。并且由模拟可知,掠入射角对成像的影响很大。对像素尺寸约10μm的探测设备,模拟得出KBA成像系统的空间分辨力上限为3μm左右。基于星光Ⅱ装置对周期为20μm的网格靶成像,获得了KBA显微镜较为清晰的X光图像。该项工作为进一步开展掠入射成像系统的研究奠定了基础。     

Determination of hydrogen sulfide and volatile thiols in air samples by mercury probe derivatization coupled with liquid chromatography-atomic fluorescence spectrometry

A new procedure is proposed for the sampling and storage of hydrogen sulphide (H₂S) and volatile thiols (methanethiol or methyl mercaptan, ethanethiol and propanethiol) for their determination by liquid chromatography. The sampling procedure is based on the trapping/pre-concentration of the analytes in alkaline aqueous solution containing an organic mercurial probe p-hydroxymercurybenzoate, HO-Hg-C₆H₄-COO⁻ (PHMB), where they are derivatized to stable PHMB complexes based on mercury-sulfur covalent bonds. PHMB complexes are separated on a C₁₈ reverse phase column, allowing their determination by liquid chromatography coupled with sequential non-selective UV-vis (DAD) and mercury specific (chemical vapor generation atomic fluorescence spectrometry, CVGAFS) on-line detectors. PHMB complexes, S(PHMB)₂CH₃S-PHMB, C₂H₅S-PHMB and C₃H₇S-PHMB, are stable alt least for 12 h at room temperature and for 3 months if stored frozen (−20 °C).The best analytical figures of merits in the optimized conditions were obtained by CVGAFS detection, with detection limits (LODc) of 9.7 μg L⁻¹ for H₂S, 13.7 μg L⁻¹ for CH₃SH, 17.7 μg L⁻¹ for C₂H₅SH and 21.7 μg L⁻¹ for C₃H₇SH in the trapping solution in form of RS-PHMB complexes, the relative standard deviation (R.S.D.) ranging between 1.0 and 1.5%, and a linear dynamic range (LDR) between 10 and 9700 μg L⁻¹. Conventional UV absorbance detectors tuned at 254 nm can be employed as well with comparable R.S.D. and LDR, but with LODc one order of magnitude higher than AFS detector and lower specificity. The sampling procedure followed by LC-DAD-CVGAFS analysis has been validated, as example, for H₂S determination by a certified gas permeation tube as a source of 3.071 ± 0.154 μg min⁻¹ of H₂S, giving a recovery of 99.8 ± 7% and it has been applied to the determination of sulfur compounds in real gas samples (biogas and the air of a plant for fractional distillation of crude oil).     

A new light emitting diode-light emitting diode portable carbon dioxide gas sensor based on an interchangeable membrane system for industrial applications

A new system for CO₂ measurement (0–100%) based on a paired emitter–detector diode arrangement as a colorimetric detection system is described. Two different configurations were tested: configuration 1 (an opposite side configuration) where a secondary inner-filter effect accounts for CO₂ sensitivity. This configuration involves the absorption of the phosphorescence emitted from a CO₂-insensitive luminophore by an acid–base indicator and configuration 2 wherein the membrane containing the luminophore is removed, simplifying the sensing membrane that now only contains the acid–base indicator. In addition, two different instrumental configurations have been studied, using a paired emitter–detector diode system, consisting of two LEDs wherein one is used as the light source (emitter) and the other is used in reverse bias mode as the light detector. The first configuration uses a green LED as emitter and a red LED as detector, whereas in the second case two identical red LEDs are used as emitter and detector. The system was characterised in terms of sensitivity, dynamic response, reproducibility, stability and temperature influence. We found that configuration 2 presented a better CO₂ response in terms of sensitivity.     

Evaluation of separation quality in two-dimensional hyphenated chromatography

In this paper, a novel criterion named the overlap index (OVI) has been proposed to evaluate the separation quality in two-dimensional hyphenated chromatography. This criterion, which is obtained from the maximum value of the Gram determinant constructed by the key spectra, can reveal the degree of two-dimensional hyphenated chromatographic separation. The key spectra are selected based on the so-called D-optimal criterion. According to its geometrical sense meaning the volume spanned by the constructed vectors, OVI criterion can practically reflect the overlap degree of chromatographic peaks. The OVI criterion is further interpreted by comparing the resolution of two-dimensional data into pure chromatograms and spectra. The successful application of this OVI criterion to both of simulated two-dimensional hyphenated data and the real case in analyzing the six reference phenolic compounds from Ginkgo biloba L-leaves shows its reliability and practicality.     

Laser absorption spectroscopy for combustion diagnosis in reactive flows: A review

Laser absorption spectroscopy (LAS) has been rapidly developed and widely applied to combustion diagnosis in recent decades. As a cost-effective tool for measuring multiple combustion parameters, LAS provides unique properties in terms of accuracy and sensitivity for understanding the reactions and kinetics in reactive flows. Line-of-sight and tomographic LAS techniques have stimulated numerous applications and been proved to be robust for in situ combustion diagnosis in uniform and non-uniform combustion fields, respectively. This review highlights the breakthroughs in the evolution of LAS techniques from the viewpoints of key principles, sensors and instrumentations developed for combustion diagnosis, with particular emphasis on a series of spatially-resolved LAS techniques with their recent applications on obtaining high-fidelity measurement results with minimal intrusion to the practical combustors. Along the way, we note some challenges and requirements for further development of the LAS-based combustion diagnosis.     

Green Determination of Total Iron in Water by Digital Image Colorimetry

A green iOS digital image colorimeter was fabricated for the determination of total iron in natural water. A mobile application operating on an iOS device was designed using Euclidean distance theory to perform iron determination. The application records the components of the color by storing red, green, and blue values as well as calculating the hue, saturation, brightness, and gray values using standard color theory. The component values obtained from the images of orange solutions of iron(II) complex with 1,10-phenanthroline were collected in a database and used for evaluation of the total iron concentration in water samples. Under the optimal conditions for solid-phase extraction used for sample preconcentration, the enrichment factor was 8.18. The iron concentration was determined by this device for concentrations from 0.01 to 1.0?ppm. The iOS digital image colorimeter achieved a limit of quantitation of 0.1?ppm. The accuracy and precision of the iOS digital image colorimeter were validated using a certified reference material, riverine water. The instrumentation was used for the analysis of natural water samples.