Synthesis and Crystal Structures of Antimony(III) Complexes With a Bis(amino)silane Ligand

Bis(amino)silane bearing bulky substituents on nitrogen, LH₂ [L = Me₂Si(NDipp)₂, Dipp = 2, 6‐diisopropylphenyl] was reacted with nBuLi (ratio 1:1 and 1:2) in toluene. The Me₂Si(LiNDipp)₂ was treated with SbCl₃ in a 1:1 ratio to yield the four‐membered SiN₂Sb ring compound of composition [η²(N,N)‐Me₂Si(NDipp)₂SbCl] ( 1 ). The mono lithiated bis(amino)silane was used to synthesize the monodentate heterotetraatomic complex [(η¹‐Me₂SiNDipp)NHDippSbCl₂] ( 2 ) by the reaction with SbCl₃. The complexes were characterized by ¹H and ¹³C NMR, elemental analysis, IR, and single‐crystal X‐ray structural analysis.     

A Luminescent Cage‐Like Complex Constructed by Bidentate Pyridine‐Containing Ligand and Silver Nitrate

The cage‐like complex, Ag₄L₄(NO₃)₄ ( 1 ) [L = 1, 4‐bis(pyridine‐2‐ylmethoxy)benzene] was synthesized by the reaction of the flexible bidentate ligand and silver nitrate. It was characterized by elemental analysis, IR spectroscopy, TG, and single‐crystal X‐ray analysis. Complex 1 is reported as the first cage‐like cluster constructed by four nitrate anions bridging two [2+2] macrocycles. A blue luminescent emission and luminescent enhancement effect are observed in complex 1 .     

Adsorption of uranium(VI) from aqueous solution by diethylenetriamine-functionalized magnetic chitosan

In this paper, the modified magnetic chitosan resin containing diethylenetriamine functional groups (DETA-MCS) was used for the adsorption of uranium ions from aqueous solutions. The influence of experimental conditions such as contact time, pH value and initial uranium(VI) concentration was studied. The Langmuir, Freundlich, Sips and Dubinin–Radushkevich equations were used to check the fitting of adsorption data to the equilibrium isotherm. The best fit for U(VI) was obtained with the Sips model. Adsorption kinetics data were tested using pseudo-first-order and pseudo-second-order models. Kinetic studies showed that the adsorption followed the pseudo-second-order kinetic model, indicating that the chemical adsorption was the rate-limiting step. The present results suggest that DETA-MCS is an adsorbent for the efficient removal of uranium(VI) from aqueous solution.     

Noncovalent Functionalization of Multiwalled Carbon Nanotubes by Anionic Polymer Poly(Sodium 4‐Styrenesulfonate) in Water

We have found that polymer poly (sodium 4‐styrenesulfonate) (PSS) is a facile and effective polymer to assist in the dispersion of MWCNTs in aqueous solutions. With the increase of the concentration of PSS solutions, the dispersibility of MWCNTs in PSS solution increases. Cast films of MWCNTs/PSS (2 wt.%) on GC electrode show a typical redox couple at scan rate of 1 V/s in phosphate buffer solution, indicating good electrical conductivity.     

LiCoO2 Hollow Nanofibers by Co‐Electrospinning Sol‐Gel Precursor

LiCoO₂ xerogel hollow nanofibers were first prepared by co‐electrospinning the sol precursor, and the polycrystalline LiCoO₂ hollow nanofibers were obtained after calcination of the xerogel fibers. The obtained hollow nanofibers made up of 20～30 nm nanocrystals were about 100 nm to several micrometers in outer diameter. The hollow nanofibers were detected by means of SEM, TEM, TG, DSC, FTIR, and XRD techniques.     

Electrospun Nickel Oxide Hollow Nanostructured Fibers

The citric acid/nickel acetate composite hollow fibers were prepared by using sol-gel processing and co-electrospinning technique. The polycrystalline NiO hollow nanostructured fibers were prepared after calcination. The obtained hollow nanostructured fibers made up of 17～25 nm nanocrystals were about 150 nm to several micrometers in outer diameter. The hollow NiO nanostructured fibers have been characterized by TG, DSC, SEM, FTIR, and XRD techniques. The results showed that the morphology of NiO hollow fibers was obviously influenced by the calcination temperature.     

两相流中煤粉的燃烧机理及动力学特征

利用微型流化床动力学分析仪研究了两相流条件下无烟煤粉的燃烧反应机理和动力学特征,并与热重法所得结果进行比较分析。结果表明,当温度大于850℃时,煤粉燃烧机理发生了变化,燃烧气态产物的生成比例也随之改变;当气速大于0.10 m/s时,气体扩散限制基本被消除,煤粉燃烧反应速率主要受界面化学反应控制;煤粉燃烧反应速率随着氧气分压的增大呈幂函数形式增长,且氧气分压对煤粉静置燃烧的影响更加显著。煤氧两相流燃烧的表观活化能与静置燃烧相比降低了49 kJ/mol,相同温度条件下两相流燃烧的界面化学反应阻力也明显小于热重法测试结果。     

湖南辰溪特高有机硫煤的稀土元素特征及其成因

采用高分辨率电感耦合等离子质谱(HR-ICP-MS)技术测定辰溪晚二叠世高有机硫(7.75%)煤中的稀土元素(REEs)。辰溪煤中∑REE变化较大,从38.84 μg/g至305.85 μg/g,加权平均值为104.57 μg/g,高于世界煤均值,与中国煤相近。辰溪煤中有明显的Ce负异常(δCe=0.74~0.84)和Eu的负异常(δEu=0.55~0.69)。煤层剖面上稀土元素含量和分布模式的变化反映了成煤环境的波动,从底板到顶板陆源物质的影响减弱,而海水的影响增强。沉积环境的阶段性变化是导致剖面上下有机硫与黄铁矿硫比值相差悬殊的原因。辰溪煤中稀土元素与铁呈现了显著的正相关性(n=11,r=0.95),说明其物质来源和富集条件有一定相似性,即陆源物质和海水共同影响的结果。稀土元素的分布模式以及∑REE与灰分、Si、Al的相关性说明了其主要来源于陆源物质;辰溪煤中δCe与δEu在剖面上变化很小,说明海水对煤中的稀土元素存在重新改造的作用。     

免疫亲和柱净化-液相色谱-串联质谱法同时测定猪肉中6种玉米赤霉醇类化合物残留量

建立了猪肉中6种玉米赤霉醇类化合物残留量的免疫亲和柱净化-液相色谱-串联质谱(IAC-LC-MS/MS)分析方法。酶解后的样品用乙醚提取,提取液浓缩后用三氯甲烷溶解,NaOH溶液反萃取,经免疫亲和柱富集和净化后,采用LC-MS/MS进行测定,外标法定量。在Shimadzu Shim-pack VP-ODS C18反相柱上分离,梯度洗脱,流动相为乙腈和2 mmol/L乙酸铵溶液;质谱采集为电喷雾负离子多反应监测模式。6种目标物的线性范围为0.5～200μg/L,相关系数(R)大于0.999,定量限(LOQ)在0.05～0.63μg/kg之间;添加浓度在1.0～5.0μg/kg范围内,方法回收率为71.3%～93.7%,相对标准偏差在3.7%～9.7%之间。该方法灵敏度高、重现性好,适用于猪肉样品中痕量玉米赤霉醇类药物残留的测定。