气相色谱法分析氯氰菊酯异构体

比较了DB-1和HP-5石英毛细管柱在不同柱流速、柱温下对氯氰菊酯异构体的分离效果,表明采用DB-1石英毛细管柱(30m×0.25mmi.d.,0.25μm)较好,柱温为240℃,柱流速为12cm/s,分析时间40min。该分析方法重现性好,分析结果准确、可靠。     

脱氢枞胺及其衍生物的研究与应用进展

脱氢枞胺及其衍生物在手性拆分、金属离子浮选、表面活性、杀菌、医药、染料等领域有着重要的用途。本文对脱氢枞胺的制备、脱氢枞胺成盐衍生物以及脱氢枞胺成键衍生物的研究与应用进展进行了综述,并对脱氢枞胺及其衍生物的研究及应用前景进行了展望。     

Fusion Domain-Adaptation CNN Driven by Images and Vibration Signals for Fault Diagnosis of Gearbox Cross-Working Conditions

The vibration signal of gearboxes contains abundant fault information, which can be used for condition monitoring. However, vibration signal is ineffective for some non-structural failures. In order to resolve this dilemma, infrared thermal images are introduced to combine with vibration signals via fusion domain-adaptation convolutional neural network (FDACNN), which can diagnose both structural and non-structural failures under various working conditions. First, the measured raw signals are converted into frequency and squared envelope spectrum to characterize the health states of the gearbox. Second, the sequences of the frequency and squared envelope spectrum are arranged into two-dimensional format, which are combined with infrared thermal images to form fusion data. Finally, the adversarial network is introduced to realize the state recognition of structural and non-structural faults in the unlabeled target domain. An experiment of gearbox test rigs was used for effectiveness validation by measuring both vibration and infrared thermal images. The results suggest that the proposed FDACNN method performs best in cross-domain fault diagnosis of gearboxes via multi-source heterogeneous data compared with the other four methods.     

Fe(Ⅳ)的合成及其稳定性研究

通过两种方法合成出Fe(Ⅳ)溶液,研究了Fe(Ⅳ)溶液的反应性、稳定性以及添加其他离子对Fe(Ⅳ)在水溶液中的稳定性的影响,并对Fe(Ⅵ)的反应历程进行了探讨。Fe(Ⅳ)离子的氧化性较Fe(Ⅵ)离子弱,可以氧化苯甲醇,而难以氧化间二甲苯;在Fe(Ⅳ)溶液中加入磷酸钠使其稳定性下降,而加入醋酸钠可显著提高Fe(Ⅳ)在溶液中的稳定性;Fe(Ⅳ)在溶液中的浓度越高越不稳定;随着碱浓度的增加Fe(Ⅳ)在溶液中的稳定性增强且在碱水溶液中Fe(Ⅳ)比Fe(Ⅵ)更稳定。     

Syndioselective propylene polymerizations by ansa-zirconocenium catalyst

The effect of reaction conditions, including catalyst concentration, temperature, and immobilization on support, have been investigated for syndioselective propylene polymerization by the “bare” zirconocenium ion generated from 1,1-diphenyl-methylidene(1-η⁵-cyclopentadienyl)(9-η⁵-fluorenyl)zirconium-dichloride precursor (2). Neither variation of the catalyst concentration nor immobilization of 2 on silica support affect the syndiospecificity of polymerization. The stereoregularity of the syndiotactic polypropylene, as judged from the melting transition temperature and homosteric r-pentad population by ¹³C-NMR, were found to be proportional to polymer molecular weight. These behaviors are compared with a typical isoselective catalyst ethylenebis(4,5,6,7-tetrahydroindenyl) Zr precursor (4). They are in close resemblance in the case of the S-enantiomeric complex of 4, but the racemic mixture of 4 is markedly inferior. The origins of stereo- and regio-errors are discussed. © 1996 John Wiley & Sons, Inc.     

Synthesis of Lanthanide–Alkylaluminium Bimetallic Complexes and Studies on Their Catalytic Activities for Polymerization of Some Polar Monomers

Three new lanthanide (Ln)–alkylaluminium (Al) bimetallic complexes with the formula [(μ-CF₃CO₂)₂Ln(μ-CF₃CHO₂)AlR₂ · 2THF]₂ (Ln=Nd, Y, R=i-C₄H₉ (i-Bu); Ln=Eu, R=C₂H₅(Et); THF=tetrahydrofuran) were synthesized by the reaction of Ln(CF₃CO₂)₃ (Ln=Nd, Y) with HAl (i-Bu)₂ and of Eu(CF₃CO₂)₃ with AlEt₃, respectively. Their crystal structures were determined by X-ray diffraction at 233 K. [(μ-CF₃CO₂)₂Nd (μ-CF₃CHO₂)Al(i-Bu)₂ · 2THF]₂ (Nd–Al) and [(μ-CF₃CO₂)₂Y(μ-CF₃CHO₂)Al(i- Bu)₂ · 2THF]₂ (Y–Al) are isomorphous and crystallize in space group P 1 with a =12.441(3) Å [12.347(5) Å for Y–Al], b =12.832(3) Å [12.832(4) Å], c =11.334(3) Å [11.292(8) Å], α=104.93 (2)° [104.45(4)°], β=98.47(2)° [98.81(4)°], γ=64.60(2)° [64.30(3)°], R =0.519 [0.113], R _w=0.0532 [0.110], Z =1 and [(μ-CF₃CO₂)₂Eu(CF₃ CHO₂)AlEt₂ · 2THF]₂(Eu–Al) in space group P 2₁/ n with a =11.913(6) Å, b =14.051(9) Å, c =17.920(9) Å, α=101.88(11)°, β=γ=90°, R =0.0509, R _w=0.0471 and Z =2. The six CF₃CO     

Effect of Cu Ions on the Dipole Moments and Polarization of Strontium Barium Niobate Single Crystals

The crystal growth, the ferroelectric hysteresis loops, and the infrared reflectivity spectra of coppermodified strontium barium niobate (SBN) single crystals are reported. Compared with the undoped SBN crystals, the copper-modified crystals have stable hysteresis loops, the spontaneous polarization of which is about 0.30 C/m², but that of the undoped SBN crystals is only about 0.12 C/m². Their coercive field strength is all about 340 V/mm. The experimental results of the infrared spectra show that the infrared reflectivities vary as the orientations of the dipole moments owing to the copper-doping. The c-axis becomes the most stable orientation of the dipole moments, and the polarization will be locked and won't recede if the copper-modified crystals are polarized into monodomains.     

How the Aggregates Determine Bound Rubber Models in Silicone Rubber? A Contrast Matching Neutron Scattering Study

The correlation between aggregates and bound rubber structures in silicone rubbers(S(phr)) with various silica fractions(ΦSi) has been investigated by contrast matching small-angle neutron scattering(SANS), swelling kinetics, and low-field nuclear magnetic resonance(NMR).Mixed solvents with deuterated cyclohexane fractions of 4.9% and 53.7% were chosen to match the scattering length densities of the matrix(SMP(phr)) and the filler(SMS(phr)), respectively. All the data consistently suggest that:(i) There is a critical threshold ΦSic between 10 and 30 phr;below ΦSic, the isolated aggregates are dominant, while beyond ΦSic, some rubber fraction is trapped among the agglomerate;(ii) ΦSiindependent thicknesses around 7.5 nm(NMR) and 8.6 nm(SANS) suggest that the bound rubber formation is determined by inherent properties of the components, and the power-law around 4.2 suggests an exponential changed gradient density of the bound rubber;(iii) SMS(80) presents a bicontinuous bound rubber with three characteristic lengths of 41, 100, and 234 nm. The expanded correlation length, a 20 nm smaller aggregate sizes suggest that such existent bicontinuous network in dry samples with less ΦSi is kind of impacted by swelling. With the obtained bound rubber models, the reinforcing mechanism of filled silicone rubber is elucidated.     

The Biological Fate of Pharmaceutical Excipient β-Cyclodextrin: Pharmacokinetics,Tissue Distribution,Excretion, and Metabolism of β-Cyclodextrin in Rats

β-cyclodextrin has a unique annular hollow ultrastructure that allows encapsulation of various poorly water-soluble drugs in the resulting cavity, thereby increasing drug stability. As a bioactive molecule, the metabolism of β-cyclodextrin is mainly completed by the flora in the colon, which can interact with API. In this study, understanding the in vivo fate of β-cyclodextrin, a LC-MS/MS method was developed to facilitate simultaneous quantitative analysis of pharmaceutical excipient β-cyclodextrin and API dextromethorphan hydrobromide. The established method had been effectively used to study the pharmacokinetics, tissue distribution, excretion, and metabolism of β-cyclodextrin after oral administration in rats. Results showed that β-cyclodextrin was almost wholly removed from rat plasma within 36 h, and high concentrations of β-cyclodextrin distributed hastily to organs with increased blood flow velocities such as the spleen, liver, and kidney after administration. The excretion of intact β-cyclodextrin to urine and feces was lower than the administration dose. It can be speculated that β-cyclodextrin metabolized to maltodextrin, which was further metabolized, absorbed, and eventually discharged in the form of CO₂ and H₂O. Results proved that β-cyclodextrin, with relative low accumulation in the body, had good safety. The results will assist further study of the design and safety evaluation of adjuvant β-cyclodextrin and promote its clinical development.     

水性颜料体系无树脂色浆的制备与应用

中性墨水属于热力学上不稳定的颜料悬浮体系,选择低黏度、高稳定性的色浆是保证墨水体系分散稳定性的重要手段之一.基于此,以颜料炭黑和酞菁蓝为着色剂,配合超分散剂(EK43)与协同增效剂(BM10),制备了两款适用于中性墨水体系的无树脂色浆.首次从色浆粒径与体系分散稳定性角度出发,确定了EK43、BM10用量以及最佳研磨时间...