固相微萃取与高效液相色谱联用技术的进展

 较全面地评述了固相微萃取与高效液相色谱联用技术的发展与应用 ,包括该技术的原理、接口装置、涂层材料等。     

合成高密度烃类燃料研究进展

本文对合成高密度烃类燃料的进展进行了总结,分别对多环烃类燃料、高张力笼状烃类燃料和添加纳米级微粒的燃料进行了评述.以烃类物质为原料,通过聚合、加氢、异构等工艺合成的多环高密度燃料拥有较高的能量密度和较佳的稳定性能,是目前高密度燃 料的发展重点.高张力笼状烃类燃料和添加纳米级微粒的燃料拥有更大的密度(一般大于1g/ cm3)和燃烧热值,是极具发展前景的新一代燃料。     

Aromatic liquid crystals with a trifluoromethyl group in the terminal chain for use in nematic LC mixtures

A new class of compounds suitable for LCD applications has have synthesized, incorporating a trifluoromethyl group in the terminal alkoxy or alkenyloxy chain. These compounds fulfil many of the specifications for use in TN-LCDs. Compounds containing several aromatic rings were synthesized with a view to producing compounds of high birefringence. This aspect also included the synthesis of compounds containing a carbon-carbon triple bond. Materials with three phenyl rings were also prepared in an attempt to produce nematic liquid crystals with a high clearing point and a high birefringence. Molecules containing a lateral fluoro substituent were synthesized in order to generate a high positive value of the dielectric anisotropy, a low melting point and no smectic mesophases. A series of compounds incorporating a carbon-carbon double bond was prepared in an attempt to produce compounds with a high nematic clearing point and a high birefringence.     

HYPERBRANCHED CONJUGATIVE MACROMOLECULES CONSTRUCTED FROM TRIPLE-BOND BUILDING BLOCKS

Polycyclotrimerization and polycoupling of acetylenic monomers respectively furnish hyperbranched polyarylenes and polyynes with high molecular weights(up to 1×10~6)in high yields(up to 99.9%).The polymers possess low intrinsic viscosities and high thermal stabilities,losing little of their weights when heated to＞400℃.Upon pyrolysis at＞800℃,the polymers graphitize with high char yields(up to 86%).Hyperbranched polyarylenes efficiently emit deep-blue to blue-green lights with fluorescence quantum yields up to 98% and strongly attenuate intense laser pulses with optical power-limiting performances superior to that of C_(60),a well-known optical lirniter.Poly(alkenephenylenes),poly(aroylarylenes)and polyynes are readily cross-linkable by UV irradiation,serving as excellent photoresist materials for the generation of patterns with nanometer resolution.Thin films of hyperbranched polyynes exhibit very high refractive indexes(n up to 1.86).The internal and terminal acetylene moieties of the polyynes readily form complexes with cobalt carbonyls,which can be transformed into soft ferromagnetic ceramics with high magnetic susceptibilities(M_s up to ca.118 emu/g)and near-zero magnetic losses.     

Parallel changes in non-photochemical quenching properties, photosynthesis and D1 levels at sudden, prolonged irradiance exposures in Ulva fasciata Delile

The photosynthetic response to a sudden and prolonged high irradiance exposure and following recovery at low irradiance were studied with the aim of investigating the ability to withstand and adapt to high irradiance without prior high light adaptation. When thalli of Ulva fasciata, accustomed to a low irradiance (80 micromol photons m(-2) s(-1)), were exposed to a high irradiance (1500 micromol photons m(-2) s(-1)), the D1 protein was rapidly degraded, reaching a steady-state level after 110 min. This was followed by a fast recovery when thalli were transferred to dim light. The overall ability of non-photochemical quenching of chlorophyll fluorescence decreased and levelled off at a sudden and prolonged exposure to high irradiance and followed the same trend as the D1 level with a fast recovery in dim light. Ulva had intrinsic means to acclimate rapidly to high irradiance, when non-photochemical quenching did not operate properly, by maintaining a smaller fraction of high light tolerant PSII assemblages and by maintaining a high non-photochemical quenching capacity of chlorophyll fluorescence in relation to the variable fluorescence. The overall absorption of light (400-700 nm) remained high during the period of high irradiance exposure. When Ulva were deprived of nutrients in the form of PES media the ability of non-photochemical quenching decreased at photoinhibitory conditions. The possible causes for the responses at prolonged irradiance and the mechanisms for the decrease of non-photochemical quenching are discussed, with implications for field measurements.     

Aromatic liquid crystals with a trifluoromethyl group in the terminal chain for use in nematic LC mixtures

A new class of compounds suitable for LCD applications has have synthesized, incorporating a trifluoromethyl group in the terminal alkoxy or alkenyloxy chain. These compounds fulfil many of the specifications for use in TN-LCDs. Compounds containing several aromatic rings were synthesized with a view to producing compounds of high birefringence. This aspect also included the synthesis of compounds containing a carbon-carbon triple bond. Materials with three phenyl rings were also prepared in an attempt to produce nematic liquid crystals with a high clearing point and a high birefringence. Molecules containing a lateral fluoro substituent were synthesized in order to generate a high positive value of the dielectric anisotropy, a low melting point and no smectic mesophases. A series of compounds incorporating a carbon-carbon double bond was prepared in an attempt to produce compounds with a high nematic clearing point and a high birefringence.     

Electrochemical Synthesis of Tetrahexahedral Rhodium Nanocrystals with Extraordinarily High Surface Energy and High Electrocatalytic Activity

Noble metal nanocrystals (NCs) enclosed with high‐index facets hold a high catalytic activity thanks to the high density of low‐coordinated step atoms that they exposed on their surface. Shape‐control synthesis of the metal NCs with high‐index facets presents a big challenge owing to the high surface energy of the NCs, and the shape control for metal Rh is even more difficult because of its extraordinarily high surface energy in comparison with Pt, Pd, and Au. The successful synthesis is presented of tetrahexahedral Rh NCs (THH Rh NCs) enclosed by {830} high‐index facets through the dynamic oxygen adsorption/desorption mediated by square‐wave potential. The results demonstrate that the THH Rh NCs exhibit greatly enhanced catalytic activity over commercial Rh black catalyst for the electrooxidation of ethanol and CO.     

Silver mirror reaction as an approach to construct superhydrophobic surfaces with high reflectivity

Superhydrophobic surfaces with high reflectivity might provide a promising self-cleaning approach in a wide variety of optical applications ranging from traffic to solar energy industries. However, the contradiction between the hierarchical micronanostructure and the high reflectivity is a challenge for superhydrophobic materials with high reflectivity. Here we report a facile method to fabricate a superhydrophobic silver film with reflectivity as high as that of polished silicon by carefully controlling the seed-induced silver mirror reaction.     

Phosphomolybdic acid-supported silica gel as efficient and cost-effective solid acid for the benzylation of indoles with benzylic alcohols

Indoles undergo smooth alkylation with benzylic alcohols on the surface of 10 mol% of phosphomolybdic acid supported on silica gel under mild conditions to produce C-3 benzylated-indoles in high yields and with high selectivity. This method offers significant advantages such as high conversions, short reaction times, mild reaction conditions, cleaner reaction profiles, high selectivity and low cost of the heterogeneous catalyst.     

A Recyclable and Scalable High-Capacity Organic Battery

Redox organic electrode materials (OEMs) have attracted extensive attention for batteries due to the possibility to be designed with high performance. However, the practical application of OEMs requires rigor criteria such as low cost, recyclability, scalability and high performance etc. and hence seems still far away. Here, we demonstrate an OEM for high performance aqueous organic batteries. Quantification of the charge storage confirmed the storage of protons with fast reaction kinetics, thereby enabling the high performance at high mass loading. As a result, the laminated pouch cells delivered Ampere-hour-scale capacity with excellent cycling performance. Benefited from the small molecular nature and the stable both charged and discharged states, the electrodes can be recycled at any states of charge with high yields (more than 90 %). This work provides a substantial step in the practical applications of OEMs for the future sustainable batteries.     

High-molar mass acrylamide-co-diacetoneacrylamide graft copolymers as viscosity enhancer for polymer flooding oil recovery

One of the most widely applied enhanced oil recovery processes is the polymer flooding, in which aqueous solution of polymer viscosifier is introduced in oil reservoirs to increase the recuperation of the remaining oil. From the current challenges of this process, it can be referred to a high cost of materials regarding their substantially required amount and the low impact on the mobility ratio during the process due to the reduction of solution viscosity at high temperatures and high salinity environments. The purpose of this study is to investigate the concept of acrylamide-based thermosassociating copolymer (TAP), with a specific morphology and chemistry (hydrophilic main backbone made of polyacrylamide with grafted amide functionalized pending chains) as viscosity enhancer at harsh conditions of high temperature and salinity. For that aim, a specific TAP microstructure was targeted (very high molar mass linear polymer chains with improved copolymer homogeneity). It is achieved in this study throughout applying the reaction engineering approach, such as synthesis in semi-batch mode or/and in heterogeneous dispersed media. As a result, the synthesized TAP presented excellent behavior as viscosity enhancer especially under high temperature and salinity conditions with improved performance in comparison to TAP synthesized by a conventional solution polymerization approach and to actual commercial high molar mass acrylamide-based polymer.     

Separation of intact proteins on γ‐ray‐induced polymethacrylate monolithic columns: A highly permeable stationary phase with high peak capacity for capillary high‐performance liquid chromatography with high‐resolution mass spectrometry

Polymethacrylate‐based monolithic capillary columns, prepared by γ‐radiation‐induced polymerization, were used to optimize the experimental conditions (nature of the organic modifiers, the content of trifluoroacetic acid and the column temperature) in the separation of nine standard proteins with different hydrophobicities and a wide range of molecular weights. Because of the excellent permeability of the monolithic columns, an ion‐pair reversed‐phase capillary liquid chromatography with high‐resolution mass spectrometry method has been developed by coupling the column directly to the mass spectrometer without a flow‐split and using a standard electrospray interface. Additionally, the high working flow and concomitant high efficiency of these columns allowed us to employ a longer column (up to 50 cm) and achieve a peak capacity value superior to 1000. This work is motivated by the need to develop new materials for high‐resolution chromatographic separation that combine chemical stability at elevated temperatures (up to 75°C) and a broad pH range, with a high peak capacity value. The advantage of the γ‐ray‐induced monolithic column lies in the batch‐to‐batch reproducibility and long‐term high‐temperature stability. Their proven high loading capacity, recovery, good selectivity and high permeability, moreover, compared well with that of a commercially available poly(styrene‐divinylbenzene) monolithic column, which confirms that such monolithic supports might facilitate analysis in proteomics.     

Tough Gel Electrolyte Using Double Polymer Network Design for the Safe,Stable Cycling of Lithium Metal Anode

The growth of lithium dendrites and low coulombic efficiency restrict the development of Li metal anodes. Polymer electrolytes are expected to be promising candidates to solve the issue, but ways to obtain a polymer electrolyte that integrates high ionic conductivity and high mechanical toughness is still challenging. By introducing a double polymer network into the electrolyte design to reshape it, a tough polymer electrolyte was developed with high conductivity, and stable operation of lithium metal anodes was further realized. The double network (DNW) gel electrolyte has high modulus of 44.3 MPa and high fracture energy of 69.5 kJ m^?2. The conductivity of DNW gel is 0.81 mS cm^?1 at 30 °C. By using this gel electrolyte design, the lithium metal electrode could be cycled more than 400 times with a coulombic efficiency (CE) as high as 96.3 % with carbonate‐based electrolytes.     

Tough Gel Electrolyte Using Double Polymer Network Design for the Safe,Stable Cycling of Lithium Metal Anode

The growth of lithium dendrites and low coulombic efficiency restrict the development of Li metal anodes. Polymer electrolytes are expected to be promising candidates to solve the issue, but ways to obtain a polymer electrolyte that integrates high ionic conductivity and high mechanical toughness is still challenging. By introducing a double polymer network into the electrolyte design to reshape it, a tough polymer electrolyte was developed with high conductivity, and stable operation of lithium metal anodes was further realized. The double network (DNW) gel electrolyte has high modulus of 44.3 MPa and high fracture energy of 69.5 kJ m⁻². The conductivity of DNW gel is 0.81 mS cm⁻¹ at 30 °C. By using this gel electrolyte design, the lithium metal electrode could be cycled more than 400 times with a coulombic efficiency (CE) as high as 96.3 % with carbonate‐based electrolytes.     

Tunable chiral monophosphines as ligands in enantioselective rhodium-catalyzed ring-opening of oxabenzonorbornadienes with amines

A new tunable chiral monophosphine was used as a ligand for asymmetric rhodium-catalyzed ring-opening of oxabenzonorbornadiene with amines, providing a series of chiral ring-opened products in high yields (up to 97%) and with high enantioselectivities (>99%).The reaction can be performed at rt to obtain the desired product with high enantioselectivity.     

Recent applications of gas chromatography with high‐resolution mass spectrometry

Gas chromatography coupled to high‐resolution mass spectrometry is a powerful analytical method that combines excellent separation power of gas chromatography with improved identification based on an accurate mass measurement. These features designate gas chromatography with high‐resolution mass spectrometry as the first choice for identification and structure elucidation of unknown volatile and semi‐volatile organic compounds. Gas chromatography with high‐resolution mass spectrometry quantitative analyses was previously focused on the determination of dioxins and related compounds using magnetic sector type analyzers, a standing requirement of many international standards. The introduction of a quadrupole high‐resolution time‐of‐flight mass analyzer broadened interest in this method and novel applications were developed, especially for multi‐target screening purposes. This review is focused on the development and the most interesting applications of gas chromatography coupled to high‐resolution mass spectrometry towards analysis of environmental matrices, biological fluids, and food safety since 2010. The main attention is paid to various approaches and applications of gas chromatography coupled to high‐resolution mass spectrometry for non‐target screening to identify contaminants and to characterize the chemical composition of environmental, food, and biological samples. The most interesting quantitative applications, where a significant contribution of gas chromatography with high‐resolution mass spectrometry over the currently used methods is expected, will be discussed as well.     

铝和铝氟病鸡模型全血骨元素和血清生化骨矿含量骨形态学的相关研究

复制了铝危害和铝氟病鸡模型。将100日龄84只雄性种鸡随机分为7个组,毒物加进配合饲料自由摄食,实验3个月。结果表明,高铝、高氟、高氟铝组在实验3周内全血多种元素和7周内的血清生化物质含量及其相关性便发生显著变化,实验13周性成熟后出现逆转并接近正常。均引骨骼元素含量、骨细胞、骨胶元、骨组织形态、骨矿代谢、骨塑形和骨骼力学机能的病理变化。性成熟后饲料加氟与未加氟各3个组的全血铁、磷、血清钙、GRT才出现分异,并与骨矿代谢动态参数的分异相吻合。表晨本实验性成熟前诸多病变主要是铝危害引起。铝可较长期使全血锌和和骨锌含量下降。全血元素含量和相关性的变化是受机体内环境影响较大的动态变化过程。骨代谢联系着广泛的生物无机化学基础。性成熟后高氟、高氟铝、高铝的危害尚有各自的特点。     

高挥发分烟煤的热解、燃烧特性研究

采用固定床热解反应器、热解 红外联用仪 (Py FTIR)和热重分析仪 ,考察了高挥发分烟煤的热解、燃烧特性 ,实验结果表明 ,高挥发分烟煤在热解过程中放出大量烃类气体 ,从燃烧试验看 ,明显分为热解段和燃烧段 ,且热解段挥发分的释放非常迅速 ,从而揭示出高挥发分烟煤燃烧过程中产生大量黑烟的原因。     

等离子体增强MOCVD法生长ZnO薄膜

利用等离子体增强MOCVD法生长出 ZnO薄膜，用X射线衍射谱观察到位于 2θ34．56°处（0002）的衍射峰，表明ZnO沿c方向呈柱状生长．通过荧光光谱，观察到来自于激子的高强度的近带边紫外光发射（375um）．紫外发射光强度与深能级复合发射光强度比高达 193，显示出材料的高质量，并通过原子力显微镜加以验证．为了实现高阻ZnO薄膜，利用高温富氧分段退火和用N2 气进行掺氮两种方法生长高阻ZnO薄膜．结果表明，电阻率由0．65 Ω·cm分别升高到1100 Ω·cm（分段退火）和5×104Ω·cm（掺氮）．进一步比较发现，掺氮的样品不仅电阻率高，而且光荧光特性好，显示出更高的薄膜质量．     

Correlation between glycated lipoproteins and fructosamine level in serum.

The correlation between the level of fructosamine and glycated proteins, including glycated lipoproteins, in serum from diabetic and nondiabetic subjects was studied. Assay of glycated proteins in serum was performed using an agarose gel film electrophoresis with nitroblue tetrazolium coloration. Glycated albumin correlated well with the fructosamine level in the diabetics (r = 0.83-0.92, p less than 0.01) but showed no correlation with the nondiabetics (r = 0.25-0.26). Also, a high correlation between the glycated beta-lipoprotein and fructosamine levels was observed in diabetic patients with hyperglycemia and in nondiabetic subjects with a high risk of atherogenesis (atherogenic index, low-density lipoprotein-cholesterol/high-density lipoprotein-cholesterol greater than 2.8) (r = 0.51-0.66, p less than 0.01). Nondiabetics with a high level of beta-lipoprotein, which is well known to cause high atherogenesity, showed a high level of glycated beta-lipoprotein similar to that in the diabetic groups with hyperglycemia; therefore, the high level of glycated beta-lipoprotein seems to be attributable not only to the hyperglycemia-accelerated glycation of beta-lipoprotein but also to an increase in the level of beta-lipoprotein in serum. Consequently, the present results show that the fructosamine level in serum reflects not only the glycation of albumin but also that of lipoproteins which are known to increase in diabetes mellitus.