ESEM-EDS: In vivo characterization of the Ni hyperaccumulator Noccaea caerulescens

Environmental scanning electron microscopy (ESEM) permits to analyze samples in their native-hydrated state, allowing a broad spectrum of biological applications. In this study, ESEM equipped with energy dispersive X-ray spectrometer (EDS) was used as a fast method to analyze tissue morphology and to investigate metal distribution in the Ni hyperaccumulator Noccaea caerulescens, an established model to study the adaptation of plants to metalliferous soils. The low vacuum and wet mode operative conditions required the proper choice of experimental parameters both for morphological and compositional characterization of plant tissues. The calibration strategy for semi-quantitative analysis involved the use of Ni fortified agar as standard and signal normalization respect to endogenous carbon, chosen as internal standard. The obtained results are in accordance with present literature, showing a preferential Ni distribution in the epidermal cells respect to near the stomata for leaves and in the cotyledon epidermidis respect to cotyledon parenchyma area for seeds. Thanks to the absence of any time consuming sample treatment steps, ESEM-EDS technique can be proposed as valid strategy for in vivo high-throughput analysis of plant tissues and for a rapid screening and identification of other hyperaccumulator plants in a selected contaminated area.     

表面等离子体共振成像生物芯片检测系统

根据表面等离子体共振(Surface Plasmon Resonance, SPR)原理,提出基于表面等离子体共振成像(Surface Plasmon Resonance imaging, SPRI)的生物芯片检测系统构建方法.介绍了SPRI生物芯片检测系统的原理、自行组建的SPRI生物芯片检测系统的结构.采用Kretschmann型棱镜耦合结构激励SPR,偏振的平行光经棱镜投射到生物芯片上,发生表面等离子体共振,由CCD摄像机采集反射光芯片图像.以巯基修饰淋病奈瑟氏菌探针为例验证该系统,利用自组装单分子层技术(Self-Assembled Monolayer,SAM)固定探针.应用该检测系统采集了探针共振、非探针处共振、探针和非探针处都不共振时的生物芯片图像.     

激光剥蚀电感耦合等离子体质谱微区分析新进展

从仪器、基础研究诸方面评述近年来LA-ICP-MS微区分析进展,重点介绍了与ICP-MS联用的激光技术发展、校正方法、分馏效应、剥蚀颗粒分布研究及仪器装置与实验技术与改进,对LA-ICP-MS技术的应用作了回顾与展望。     

Electron probe microanalysis of SiO2-coated minerals: Subsurface phases in quartz

Crystal fragments of biotite, garnet, and spinel were mounted together in one block which afterwards was sawn into several pieces; each piece was coated with SiO₂ of varying thickness, up to 7.9m. Electron probe microanalysis was carried out at various accelerating voltages of the major elements present, using the non-SiO₂-coated minerals as reference standard.Calibration curves, depth below the surface versus ratios of X-ray yields, have been established with the ultimate goal to use them for a (semi)-quantification of elements present in subsurface phases in quartz, a common host mineral in rocks.     

Microchemical and Microstructural Characterization of the Early Stages of the Discontinuous Precipitation Reaction in Al-22 at.% Zn Alloy

High-spatial energy dispersive X-ray (EDX) microanalysis has been applied in order to reveal changes of chemical composition accompanying the formation of the lamellar structure due to discontinuous precipitation reaction in Al-22at.% Zn alloy. The line-scans performed in the reaction zone have shown that the region left behind the grain boundary (GB) after its displacement from the original position is solute depleted, similar to the de-alloying case of diffusion induced grain boundary migration. This enables the allotriomorphs to be transformed into solute-rich lamellae and development of lamellar + structure, especially if the GB moves in the direction perpendicular to its original location. If the direction of movement is strongly inclined to the original location of the GB, the growth usually stops after a short period of time, mainly due to formation of the precipitation free zone (PFZ) ahead of the reaction front. The detailed EDX examination revealed that there is a sharp change in solute content at the lamella/PFZ and PFZ/matrix alloy interfaces. The solute content in the PFZ is lower than in the neighbouring lamella and it corresponds to the equilibrium state. Therefore, one can suppose that the PFZ is formed due to backward movement of the reaction front in order to consume the excess of solute atoms stored in the lamellae in comparison with the equilibrium state. As soon as the equilibrium state is attained within the PFZ, the growth of the colony is completed.     

Analytical Electron Microscopy Examination of the γ′/γ Interfaces in a Ni-Based Superalloy

The investigation of microstructure and chemical composition of the and phases were performed in a Ni-base superalloy by means of analytical electron microscopy. The distribution of particular elements in the alloy was revealed using X-ray mapping in a transmission electron microscope. The detected concentration profiles of alloying elements at the / interface were relatively sharp in the case of cuboidal shape of the phase while they resembled the classical diffusion profile for the oval phase. The quantitative analysis of the phase revealed much higher content of Al and lower of Ti, W, Co and Mo in the oval precipitates compared to cuboidal ones. This result is attributed to the different solidification paths, which is eutectic for the cuboidal precipitates and peritectic for the oval precipitates.     

固定化脂肪酶活性的X射线微区分析

利用X射线微区分析的方法，对吸附交联法得到的固定化脂肪酶的微观活性进行了分析。结果表明：以合成出的大孔吸附树脂为固定化酶栽体，酶活较高，活性脂肪酶分布较均匀。并得到了固定化脂肪酶的活性定位的最佳条件。     

Determination of 25 elements in the complex oxide mineral zirconolite by analytical electron microscopy

In this paper we describe a technique for the determination of 25 elements in natural zirconolite using energy-dispersive analytical electron microscopy (AEM). The method presented here allows one to quantitatively investigate the chemistry of submicron-scale zones in complex oxide minerals. The effects of electron channeling, thickness variability and variations in detector resolution were minimized by using a controlled set of operating procedures and instrument parameters. To provide a high level of accurayy, k_ATI-factors were determined from standards for most of the 25 elements of interest, including all of the major elements. Each analytical spectrum is reduced to a set of raw peak counts (and errors) using a digital top-hat filter to suppress background followed by multiple least squares fitting of reference spectra. Counting times of 12–15 min per analysis were required to provide suitable counting statistics. Results are presented for zirconolite samples from the contact metamorphic aureole of the Bergell granodiorite intrusion, Switzerland-Italy. A comparison of 43 AEM analyses with 15 analyses obtained by wavelength-dispersive electron probe microanalysis (EPMA) shows that there is excellent agreement between the two data sets in the amounts of individual elements present, chemical trends and overall stoichiometry. An assessment of the combined data set shows that the major substitution mechanisms in the Bergell samples are coupled substitutions involving the M5,6- and M8-sites of the zirconolite structure: ^M8Ca²⁺ + ^M5,6Ti⁴⁺→^M8REE³⁺ + ^M5,6(Al,Fe)³⁺ and ^M8Ca²⁺ + ^M5,6Ti⁴⁺→^M8(Th,U)⁴⁺ + ^M5,6 (Mg,Fe)²⁺.