2,2,6,6-四甲基哌啶-1-氧自由基促进的钒基催化剂催化苯直接氧化制苯酚

以钒基化合物为催化剂,在TEMPO(2,2,6,6-四甲基哌啶-1-氧自由基)存在下,能形成快速催化分子氧氧化苯制苯酚的催化体系.在反应过程中,由类似芬顿试剂反应过程生成的羟基自由基亲核进攻苯环,形成羟基环己二烯自由基;该羟基氢可在TEMPO存在的催化体系中消除,同时苯环氢可立即转移至氧原子而生成苯酚.在以[(CH3)...     

LIF技术测量浓度场的影响因素分析

本文研究了作为示踪剂的荧光素钠的谱图，测定了荧光素钠在蒸馏水和普通自来水中的吸光系数，估算了荧光分子的平均寿命。最后，详细分析了浓度、激光功率、温度、ｐＨ值和截止滤光片对荧光强度的影响。     

均匀棒状过氧化氢合碳酸钠制备及非等温热分解动力学

本文制备了均匀棒状过氧化氢合碳酸钠，化学分析确定其组成为Na₂CO₃·1.5H₂O₂，用DTA-TG-DTG技术并辅以X-ray分析研究了它在静态空气、流动氧气和流动氮气气氛中的非等温热分解过程及动力学。     

基于长脉冲光源的钠信标回光特性实验研究

采用与信标发射接收系统参数匹配的长脉冲光源,可在脉冲回光时间内产生较亮星等的钠信标,既有利于提高信标探测的信噪比,也有利于实现自适应光学系统的高频闭环校正.基于450 mm直径望远镜和大能量长脉冲光源,开展了钠信标探测实验,得到了长脉冲光源产生的钠信标回光特性.通过CCD和光电倍增管,采集得到了不同发射能量、出射偏振态下的回光强度,并获得了最大强度为15万光子/m2/pulse的回光,对应脉冲回光时间内约4.1等星的亮度.分析推算了实验条件下钠原子的柱密度.实验全过程未出现明显的饱和现象,验证了采用长脉冲钠信标光源避免饱和效应、得到高亮度钠信标的可行性.     

选择性氧化含氰基的对硝基苯硫醚

选择性氧化含氰基的对硝基苯硫醚岳国仁，王建华，张正（南京大学化学系南京２１０００８）关键词含氰基硫醚，选择性氧化，四水合过硼酸钠据报道［１］对硝基苯磺酰基乙腈的合成，反应时间长，可采用四水合过硼酸钠（ＮａＢＯ３·４Ｈ２Ｏ）作为氧化剂，受到重视［２，３...     

一种规整单壁碳纳米笼的合成与改性及其对水体结晶紫分子的吸附性能

运用催化气相沉积法及继之的纯化处理,获得了具有规整外型、中空及密集阵列的单壁三维结构碳纳米笼(carbon nanocages,CNCs)。尝试将其用于水体阳离子染料结晶紫(crystal violet,CV)的吸附去除,实验条件下其上CV的饱和吸附容量可达542.6 mg·g~(-1)。进一步以十二烷基苯磺酸钠(sodium dodecyl benzene sulfonate,SDBS)对制得的CNCs表面进行亲水性改性,观察到了改性CNCs对CV吸附性能的明显提升,相同条件下其上CV的饱和吸附容量显著提升至748.5 mg·g~(-1)。运用多种表征及测定,探明改性前后CNCs的组成和结构,并尝试与其吸附性能关联,在此基础上探明改性及促进机制,为进一步研发具有实用意义的污水处理技术提供有益参考。     

Certified reference material for the determination of perfluorooctane sulfonate in acrylonitrile-butadiene-styrene resin (NMIJ CRM 8155-a)

A certified reference material (CRM) for the determination of perfluorooctane sulfonate (PFOS) in acrylonitrile-butadiene-styrene (ABS) resin (NMIJ CRM 8155-a) has been issued by the National Metrology Institute of Japan (NMIJ). The bulk material was prepared by mixing commercial ABS resin powder and potassium PFOS and cut into square plates (20 × 20 mm, 2 mm thick) as the CRM. Analytical processes combined with isotope-dilution mass spectrometry and liquid chromatography/mass spectrometry were optimised and applied for characterisation. One of the approaches adopted by NMIJ for certification is that results from two or more primary methods of measurement should be used; thus, two optimised isotope-dilution mass spectrometric methods (Methods 1 and 2 with reprecipitation and with reprecipitation/solid phase extraction, respectively, were validated mutually and employed) were used to determine the certified value. Homogeneity and stability of the square plates were evaluated and their uncertainty contributions (as relative standard uncertainties) were 1.43% for inhomogeneity and 6.96% for approximately two years’ instability. The certified mass fraction of linear PFOS (heptadecafluoro-1-octanesulfonic acid) in the CRM with expanded uncertainty (coverage factor k = 2, approximately 95% confidence interval) was (33.1 ± 5.0) mg kg^?1 as free acid of PFOS.     

Reduction of N,N‐Dimethylcarboxamides to Aldehydes by Sodium Hydride–Iodide Composite

A new and concise protocol for selective reduction of N,N‐dimethylamides into aldehydes was established using sodium hydride (NaH) in the presence of sodium iodide (NaI) under mild reaction conditions. The present protocol with the NaH‐NaI composite allows for reduction of not only aromatic and heteroaromatic but also aliphatic N,N‐dimethylamides with wide substituent compatibility. Retention of α‐chirality in the reduction of α‐enantioriched amides was accomplished. Use of sodium deuteride (NaD) offers a new step‐economical alternative to prepare deuterated aldehydes with high deuterium incorporation rate. The NaH‐NaI composite exhibits unique chemoselectivity for reduction of N,N‐dimethylamides over ketones.     

Synthesis and crystal structure of a polymeric erbium(III)–sodium(I) coordination complex of picolinic acid N-oxide

A new Er(III)–Na(I) coordination polymer of stoichiometry [NaEr₂L₅(H₂O)₆(NO₃)](NO₃)·3.5H₂O (HL = picolinic acid N-oxide) has been synthesized and characterized by single-crystal X-ray analysis. Crystals are triclinic, P with a = 9.823(2), b = 12.453(2), c = 20.643(4) Å; = 98.49(3), ( = 101.40(3), = 108.69(3)°; V = 2284(1) ų; Z = 2. Of the two independent eight-coordinate erbium(III) ions in this complex, one is surrounded by four bidentate chelating L ligands, and the other by one bidentate chelating L ligand, four aqua ligands and two anti-carboxylate oxygen atoms from two neighboring [ErL₄] units. The sodium(I) ion is in a distorted octahedral environment, being coordinated by a unidentate nitrate anion, three aqua ligands and two anti-carboxylate oxygen atoms from two adjacent [ErL₄] units. The complex is built from zigzag chains of syn-anti carboxylate-bridged erbium(III) moieties directed in the a direction, which are cross-linked pairwise by aqua-bridgeddimericsodium(I) units. The resulting composite polymeric chains are further connected by hydrogen bonds to form a three-dimensional network.     

Crystal structure of aquo (hydroxo) (ethylenediaminetetraacetato) sodium(I) tin(IV), NaSn(OH)(edta)(H2O)

NaSn(OH)(edta)(H₂O) is monoclinic, space groupP2₁/c, witha=9.747(3)Å,b=9.121(3)Å,c=16.430(6)Å, =98.69(4)°, ų, andZ=4. The coordination environment of Sn(IV) is a capped octahedron. Sn–O distances range from 1.990(6)Å to 2.351(7)Å. Na(I) is five coordinated to three different edta molecules. Na–O distances range from 2.283(9)Å to 2.414(7)Å. The edta ligand presents the E, G/R conformation. The crystal structure is composed of sheets parallel to (001): inside a sheet Sn(OH)(edta) molecules are connected to each other by the Na(I) interactions.