Synthesis,crystal structures and electrochemical properties of group 6 metal carbonyl anion complexes

A series of [M(CO)₅I]⁻ and [M₂(CO)₁₀I]⁻ anion complexes have been synthesized by the photochemical reaction of PhCH₂N(CH₃)₃I or FcCH₂N(CH₃)₃I (Fc=ferrocenyl) with M(CO)₆ (M = Cr, Mo or W), and characterized by elemental analyses, i.r., ¹H-n.m.r. and ¹³C-n.m.r. spectra in the case of the molybdenum and tungsten complexes. These complexes exhibit considerably different electrochemical behavior, when investigated by cyclic voltammetry. The crystal structures of [PhCH₂N(CH₃)₃][Cr(CO)₅I] and [FcCH₂N(CH₃)₃][W₂(CO)₁₀I] have been determined by X-ray diffraction, indicating that only weak contacts maybe exist between anions and cations by the I...H bond in the former, and there are no direct interactions between anions and cations in the latter.     

超高效液相色谱-串联质谱法测定白芷中51种禁用农药的残留量

将白芷药材粉碎至通过孔径为(250±9.9)μm的网筛,并称取此白芷粉末样品2.00g于聚丙烯管中与水10mL混匀,再加入含1%(体积分数)乙酸的乙腈10.0mL,涡旋1min后加入无水硫酸镁4g和乙酸钠1g,剧烈振荡3min,离心5min,取其上清液5.0mL置于已盛有无水硫酸镁900mg、N-丙基乙二胺(PSA)450mg和硅胶300mg的净化管中,剧烈振荡5min使净化完全,离心5min。移取上清液3.0mL于40℃水浴中减压蒸缩至近干。加入50μg·L^-1的磷酸三苯酯内标溶液300μL,加入乙腈定容至1.0mL,经0.20μm滤膜过滤,取其滤液,按仪器工作条件进行超高效液相色谱-串联质谱法分析。选用Eclipse Plus C18色谱柱和以不同比例的(A)含10mmol·L^-1甲酸铵的0.1%(体积分数)甲酸溶液和(B)乙腈的混合液为流动相,按梯度洗脱程序对白芷中可能残留的51种禁用农药进行色谱分离,并在电喷雾离子源正、负离子(ESI+和ESI-)电离方式和动态多反应监测(dMRM)模式条件下进行串联质谱法测定。采用基质匹配标准曲线法定量。51种农药的质量浓度在一定范围内与其对应的峰面积呈线性关系,并测得其检出限(3S/N)为0.3~5.0μg·kg^-1。标准加入法回收试验的结果显示,其中大部分农药的回收率在71%以上,测定值的相对标准偏差(n=6)均小于20%。按此方法分析了70批白芷样品,共检出16种农药,其中甲拌磷亚砜的检出率达95%,最高检出量为15.2μg·kg^-1;甲拌磷砜和毒死蜱的检出率均为10%,最高检出量依次为3.5,45.0μg·kg^-1,其余13种农药的检出率均低于5%,且检出量均较低。     

A Novel Method for the Determination of Fungicide Residues in Tobacco by Ultra-performance Liquid Chromatography–Tandem Mass Spectrometry Combined with Pass-Through Solid-Phase Extraction

Chromatographia - A novel method for the rapid simultaneous determination of multiple fungicide residues in tobacco was established using ultra-performance liquid chromatography–tandem mass...     

Automatic hierarchy classification in venation networks using directional morphological filtering for hierarchical structure traits extraction

The extraction of vein traits from venation networks is of great significance to the development of a variety of research fields, such as evolutionary biology. However, traditional studies normally target to the extraction of reticulate structure traits (ReSTs), which is not sufficient enough to distinguish the difference between vein orders. For hierarchical structure traits (HiSTs), only a few tools have made attempts with human assistance, and obviously are not practical for large-scale traits extraction. Thus, there is a necessity to develop the method of automated vein hierarchy classification, raising a new challenge yet to be addressed. We propose a novel vein hierarchy classification method based on directional morphological filtering to automatically classify vein orders. Different from traditional methods, our method classify vein orders from highly dense venation networks for the extraction of traits with ecological significance. To the best of our knowledge, this is the first attempt to automatically classify vein hierarchy. To evaluate the performance of our method, we prepare a soybean transmission image dataset (STID) composed of 1200 soybean leaf images and the vein orders of these leaves are manually coarsely annotated by experts as ground truth. We apply our method to classify vein orders of each leaf in the dataset. Compared with ground truth, the proposed method achieves great performance, while the average deviation on major vein is less than 5 pixels and the average completeness on second-order veins reaches 54.28%.     

Novel CD-MOF NIR-II fluorophores for gastric ulcer imaging

Gastric ulcers are one of the most common stomach diseases that often accompanied by inflammation, congestion, edema, scar tissue formation, and pyloric obstruction. Fiberoptic endoscopy and X-ray analysis of the upper GI tract have become the diagnostic procedure of choice for patients. However, conventional diagnosis technology is either invasive or radioactive. Herein, a novel CD-MOF NIR-II fluorophore (GPs-CH1055) was developed. The relative fluorophore intensity was largely consistent at various media and pH buffers, and it can swell into gel particles in solvents and be completely expelled from the gastrointestinal tract without being assimilated. GPs-CH1055 has been further evaluated in vivo, and exhibited strong retention effect on the gastric ulcer sites, bright NIR-II signals with high spatial and temporal resolution. Therefore, GPs-CH1055 shows great promise for realizing real-time gastric ulcer imaging and diagnosis.     

HG-AFS测定西藏日多温泉水中砷的形态

本文采用氢化物发生-原子荧光光谱法(HG-AFS)测定温泉水中砷的形态,重点研究了西藏温泉水中砷的存在形态,发现水中除常见的砷酸盐[砷(Ⅴ)]、亚砷酸盐[砷(Ⅲ)]和有机砷外,还存在悬浮态砷。实验结果表明,西藏温泉水中砷的形态分布呈现出五价砷>三价砷>悬浮态砷>有机砷的特征,讨论了各形态态砷的相互影响因素,为进一步开发利用西藏温泉提供了科学依据。     

Multilayer dielectric cylindrical mirrors based on omnidirectional reflection from a one-dimensional photonic crystal

A multilayer dielectric cylindrical mirror (MDCM) based on the one-dimensional omnidirectional reflection of a photonic crystal is presented. In this case, the refractive indices of the two materials are 1.6 (polystyrene) and 4.6 (tellurium), and the corresponding optimized thicknesses are 0.75a and 0.25a. A very high reflectance over a wide frequency range is observed. In this case, a is the lattice constant of the photonic crystal. In this band, the MDCM has good reflection and focal properties. Therefore, it is feasible to use the MDCM for integrated waveguide devices. As an example, an etched diffraction grating demultiplexer based on the MDCM is also proposed. Both the operational principle and design of the device are introduced. This provides a method for designing compact integrated waveguide devices.     

浅析量子力学中的不确定性原理

德国物理学家海森伯在1927年提出的不确定性原理,包括两力学量间的不确定性原理和能量与时间的不确定性原理,它的提出意味着量子力学不仅有了完整的数学形式,而且有了合理的理论解释.本文尝试通过对不确定性原理的创立背景、过程、应用等来对这一原理做简要介绍,特别强调了科学讨论在科学发展中的作用.     

Combined ultrasound and germination treatment on the fine structure of highland barley starch

Highland barley is a grain crop grown in Tibet, China. This study investigated the structure of highland barley starch using ultrasound (40 kHz, 40 min, 165.5 W) and germination treatments (30℃ with 80% relative humidity). The macroscopic morphology and the barley's fine and molecular structure were evaluated. After sequential ultrasound pretreatment and germination, a significant difference in moisture content and surface roughness was noted between highland barley and the other groups. All test groups showed an increased particle size distribution range with increasing germination time. FTIR results also indicated that after sequential ultrasound pretreatment and germination, the absorption intensity of the intramolecular hydroxyl (–OH) group of starch increased, and hydrogen bonding was stronger compared to the untreated germinated sample. In addition, XRD analysis revealed that starch crystallinity increased following sequential ultrasound treatment and germination, but a-type of crystallinity remained after sonication. Further, the Mw of sequential ultrasound pretreatment and germination at any time is higher than that of sequential germination and ultrasound. As a result of sequential ultrasound pretreatment and germination, changes in the content of chain length of barley starch were consistent with germination alone. At the same time, the average degree of polymerisation (DP) fluctuated slightly. Lastly, the starch was modified during the sonication process, either prior to or following sonication. Pretreatment with ultrasound illustrated a more profound effect on barley starch than sequential germination and ultrasound treatment. In conclusion, these results indicate that sequential ultrasound pretreatment and germination improve the fine structure of highland barley starch.     

In-depth study of the sulfur migration and transformation during hydrothermal carbonization of sewage sludge

This study investigated the effect of temperature on sulfur transformation behavior during the hydrothermal carbonization of raw sludge, water washed sludge and the corresponding filtrate solution at 110–235 °C. The different sulfur species in the various products were determined, primarily focusing on the sulfur species present in the aqueous product. At 110 °C, 31.9% of sulfur migrated to the aqueous product, primarily in the form of sulfone-S and sulfoxide-S. As the temperature increased to 160 °C, the hydrolysis of aliphatic-S and aromatic-S was enhanced, and the former species further transformed to other organic-S or SO₄²-S in the aqueous product. High temperature is beneficial to the formation of sulfate-S and thiophene-S/aromatic-S in the aqueous and hydrochar products, along with the release of H₂S and CH₃SH. This caused a retention of only 29.2% sulfur (i.e., sulfate-S) in the hydrochar at 235 °C, with a large amount of sulfur migrating to the aqueous product (51.1%), followed by the gas product (9.1%). Among all the sulfur species in raw sludge, aliphatic-S was the most thermally unstable. SO₄²-S and sulfur-containing gas were primarily formed from the decomposition of water-insoluble aliphatic-S, while part of thiophene-S/aromatic-S in aqueous products was generated from water-soluble sulfone-S and sulfoxide-S at high temperatures of ≥160 °C. The results indicate that 210 °C is the optimal temperature for preparing of sludge-based fuel during hydrothermal carbonization, and water washing pre-treatment is a good strategy for enhancing the removal of sulfur in hydrochar and reducing the release of sulfur-containing odorous gas.