The effects of washing a collagen sample prior to TEM examination

Transmission electron microscopy (TEM) is an important analysis technique to visualize (bio)macromolecules and their assemblies, including collagen fibers. Many protocols for TEM sample preparation of collagen involve one or more washing steps to remove excess salts from the dispersion that could hamper analysis when dried on a TEM grid. Such protocols are not standardized and washing times as well as washing solvents vary from procedure to procedure, with each research group typically having their own protocol. Here, we investigate the influence of washing with water, ethanol, but also methanol and 2-propanol, for both mineralized and unmineralized collagen samples via a protocol based on centrifugation. Washing with water maintains the hydrated collagen structure and the characteristic banding pattern can be clearly observed. Conversely, washing with ethanol results in dehydration of the fibrils, often leading to aggregation of the fibers and a less obvious banding pattern, already within 1 min of ethanol exposure. As we show, this process is fully reversible. Similar observations were made for methanol and propanol. Based on these results, a standardized washing protocol for collagenous samples is proposed.     

Effect of focused ion beam sample preparation on the phase composition of zirconia

The investigation of phase transformations in metastable ceramic systems such as zirconia often requires local phase analysis within the areas of interest. Electron backscatter diffraction is a suitable method in combination with focused ion beam sample preparation. The interaction between ion beam and sample has to be carefully considered. In case of metastable Y-PSZ and Mg-PSZ, phase transformations were observed after FIB preparation with 30?kV, 30?nA and 5° incidence angle. Damage was the dominating effect for angles of 72°. The expected local temperature increase due to the ion bombardment with 30?kV and 30?nA is 700?K for ZrO₂. Thus, the observed phase transformations can be explained on the basis of the temperature increase in the corresponding Y-PSZ phase diagram. In case of Mg-PSZ, the transition temperature is 1083?°C. The local temperature increase was obviously lower. The excitation energy for the observed phase transformation was smaller than expected from the phase diagrams of the thermodynamic equilibrium. Using 5?kV, 4.8?nA and 5° incidence angle, no phase transformations and no damage were observed. Thus, these conditions are well suited for the FIB preparation of metastable zirconia.     

直接氯化法合成对硝基氯化苄

介绍了以对硝基甲苯和氯气为原料 ,在催化剂存在下合成对硝基氯化苄的方法 ,考察了催化剂种类、反应温度、溶剂配比等因素对反应的影响 ,优化的反应条件为 :对硝基甲苯用量 1 3 7g,对硝基甲苯 /邻二氯苯 (摩尔比 ) =1∶ 0 .6,w (偶氮二异丁腈 ) =0 .6% ,反应时间 3 h,反应温度 1 60℃ ,产物单程收率大于 65 % ;将反应混合物中未反应的原料分离后 ,以无水乙醇为溶剂结晶纯化 ,物料 /溶剂 (摩尔比 ) =1∶ 1 .5时晶体含量在 99.0 %以上 ,结晶收率达 67     

A procedure to prepare cross-sectional samples for TEM

Cross-sectional transmission electron microscopy (XTEM) is an imaging technique particularly suited to the study of layered structures. For integrated electronic devices it has become a common practice to use XTEM to assess the shape and crystallinity of component layers as well as defect structures introduced by processing. A procedure for preparing samples to be viewed by XTEM is described.     

2-环戊基环戊酮香料的制备与应用

以尼龙酸副产物2-亚环戊基环戊酮为原料，液体镍为催化剂，催化加氢制得了2-环戊基环戊酮。经元素分析、GCMS、IR、^1HNMR、^13C NMR检测，认为结构正确，色谱纯度大于99．9％。大鼠口服LD50雄性5381．5mg／kg，雌性5087．5mg／kg。具有留兰香样的香气，可用作食用和日用香料。     

Preparation of Plate Fe_(60)Co_8Zr_(10)Mo_5W_2B_(15) Bulk Amorphous Alloy and Its Fracture Toughness

1Introduction Duwez[1]synthesizedthefoilAu Siamorphousalloyforthefirsttimewithrapidsolidification,whichinitiatedthepreparationofamorphousalloysintheprocessofalloysolidification,andthereaftertheresearchonamorphousal loysdevelopedrapidly.Since1980s,withthec…     

Low temperature synthesis of aluminium titanate by an aqueous sol-gel route

Formation of aluminium titanate (AT) has been achieved at low temperature through sol-gel process using boehmite and titanium hydroxide as precursors by controlling the particle size at nanoscale followed by in-situ peptisation. The formations of AT phase, particle size distributions, sintering and thermal expansion characteristics, and microstructural features have been reported. DTA and XRD analysis have been performed to confirm the formation of AT. A 94% relative density was obtained for aluminium titanate sintered at 1550 °C with controlled grain size in the range of 2-3 μm.     

Preparation and Characterization of Starch-g-PVA/Nano-hydroxyapatite Complex Hydrogel

1Introduction Biodegradablehydrogelshadattractedmuchattentioninrecentyearsduetotheiruniquecombinationofproper ties,suchasbiocompatibility,permeability,hydrophilici ty,andlowcoefficientoffriction[1].Poly(vinylalcohol)(PVA)waswater solubleanddegradable[2].I…