Surface functionalization of ordered mesoporous carbons--a comparative study

Hexagonally structured mesoporous carbons C15 and CMK-5 and cubically structured carbon C48 were synthesized using ordered silica SBA-15 and MCM-48 as templates and carbon precursors of different structures. The surfaces of these ordered carbons were chemically functionalized by employing an approach, in which the selected diazonium compounds were in situ generated and reacted with the carbon frameworks of the mesoporous carbons. The aromatic organic molecules containing chlorine, ester, and alkyl groups were covalently attached to the surface of these ordered mesoporous carbons. The presence of functional groups on the modified carbons was confirmed with Fourier transform infrared spectroscopy, thermogravimetric analysis, and nitrogen adsorption. The BET-specific surface area and the pore width of ordered carbons were significantly reduced, whereas the primary structure of these ordered carbons and their unit cells were intact. Basically, the density of grafted functional groups is related to the specific surface area of the sample, particularly the surface area of mesopores. The surface functionalization reaction takes place only on the external surface of carbon C15, while it occurs on both of the internal and external surface of CMK-5 carbon with the nanopipe structure. The presence of the micropores in CMK-5 carbon should be responsible for its lower grafting density because the small micropores are inaccessible in the reaction. It was also proposed that the preferred adsorption/reaction in C48 may be related to the observed unsymmetrical degradation of the XRD patterns for the functionalized C48 samples. The chemical modification process considerably reduced the primary mesopores in these ordered carbons by approximately 1-1.5 nm, affording carbons with micropores in the cases of C15 and C48, and mixed micropores and small mesopores in the case of CMK-5. A grafting density of approximately 0.9-1.5 micromol/m(2) was achieved under current research.     

水热微乳液法合成BaLiF3∶Er3+纳米微粒及表征

采用水/CTAB/正丁醇/正辛烷体系微乳液法及水热技术制备了BaLiF3∶Er3+纳米微粒.利用X射线衍射(XRD)、环境扫描电镜(ESEM)和红外荧光光谱等手段对所制备产物进行了表征.X射线衍射数据表明, 所制备微粒与JCPDS 标准卡片18-715吻合很好, 利用谢乐公式计算所制备产物平均粒径在98.45 nm左右, 与环境扫描电镜观察结果基本相同.BaLiF3∶Er3+纳米微粒的红外发射图谱由4个峰构成, 最强峰位于1540 nm处, 属于Er3+的f→f跃迁.     

Effects of Oxygen and Water Vapor on Volatile Organic Compounds Decomposition Using Gliding Arc Gas Discharge

The combined effects of oxygen and water vapor on three typical volatile organic compounds, i.e. tetrachloromethane, n-butane and toluene, decomposition efficiency under gliding arc gas discharge conditions are studied. The electron density and the density of the reactive radicals such as O and OH are modified by addition of oxygen and water vapor. Consequently, the decomposition process can be enhanced or suppressed, depending on the involved chemical structures and reaction channels. The addition of oxygen and water vapor suppresses the tetrachloromethane decomposition which indicates that this process is mainly controlled by the electron dissociation reactions. By contrast, the n-butane and toluene decompositions are enhanced, which shows that they can be mainly ascribed to the radical induced reactions. Especially, in a moist atmosphere the OH radicals are supposed to play the most important role in the n-butane decomposition process.     

Gear-like array of (H_2O)_(12) as building blocks in one-dimensional supramolecular assembly

The preparation and crystal structure of complex Co(Hsae)_2·2H_2O (1,H_2sae=N-salicylidene-2-iminoethanol) are reported.X- ray analysis revealed that every six Co(Hsae)_2 forms a cyclic chip and every 12 water forms a novel gear-like cluster.Acting as building blocks,the gear-like water cluster and complex chip are connected in A-B fashion and extend into one-dimensional supramolecular chain.Hydrogen bond is the primary bridging force in the formation of supramolecular framework.     

高强度聚乙烯醇/聚苯胺/聚吡咯/TiO2导电杂化水凝胶的制备与性能

本文以聚乙烯醇(PVA)、苯胺(ANI)、吡咯(Py)及钛酸丁酯(TBOT)为原料,通过溶胶-凝胶法、原位氧化聚合法及冷冻-融溶法一步得到聚乙烯醇/聚苯胺/聚吡咯/TiO 2(PVA/PANI/PPy/TiO 2)杂化水凝胶。结果表明,该杂化水凝胶具有优异的力学性能和导电性能。当n(ANI)∶[KG-*3/5]n(Py)=8∶[KG-*3/5]2(TBOT体积为100μL)时,其压缩强度高达2.45 MPa。同时,在外加电源的作用下,该凝胶能够使灯泡发光。当n(ANI)∶[KG-*3/5]n(Py)=2∶[KG-*3/5]8(TBOT体积为150μL)时,杂化水凝胶的电导率(0.25 S/m)最好。该杂化水凝胶有望广泛地应用在柔性可穿戴电子器件、安全离子电池、传感器和生物器件等领域。     

Pulse radiolysis of one-electron oxidation of rare tricyclic nucleoside derivative

~~Pulse radiolysis of one-electron oxidation of rare tricyclic nucleoside derivative@赵红卫$Shanghai Institute of Nuclear Research, Chinese Academy of Sciences! Shanghai 201800,China @江致勤$Department of Chemistry, Tongji Unviersity!Shanghai 200092,China @窦大营$Shanghai Institute of Nuclear Research, Chinese Academy of Sciences! Shanghai 201800,China @吴铁一$Shanghai Institute of Nuclear Research, Chinese Academy of Sciences! Shanghai 201800,China @王文锋$Shanghai…     

Determination of Dopamine in the Presence of Ascorbic Acid on the IrO2-Ta2O5 Type DSA Electrode

IrO2Ta2O5 (70%: 30%, molar ratio) electrodes (ITEs) were prepared by the thermal decomposition method. Typical “mud-cracked” surface and surface enrichment of Ta were observed. The determination of dopamine (DA) was carried out in the presence of ascorbic acid (AA). The detection limit of DA was 5~10 5 mol/L without the interference of AA.     

Development of an analytical procedure for determination of selected estrogens and progestagens in water samples

An analytical procedure has been developed for determination of eight selected natural and synthetic hormonal steroids in surface water and in effluent samples. Several methodological points have been investigated and are discussed; they include the choice of the solid-phase extraction sorbent, the influence of flow rate on recovery, the breakthrough volume for a given sorbent (Env+ and Oasis HLB), sample clean up, and sample storage. As regards the latter point, it was found that when no preservative was added to effluent from a sewage-treatment plant, severe loss of steroids occurred—85% of progesterone and about 30% of both estrone and estradiol were found to be degraded in 24 h. The procedure developed was applied to samples from the Seine river estuary. Sex steroids were not detected in surface water; estrone was the most commonly detected steroid in sewage-treatment plant effluent, with levels ranging from 1.8 to 8.3 ng L^–1. Synthetic estrogens (ethynylestradiol and mestranol) and progestagens (levonorgestrel and norethindrone) were never detected, whatever the sampling season. Overall, for 162 out of 168 measurements levels were below the detection limits of the developed procedure.     

络合滴定法测定钙含量微型实验研究

利用微型滴定法测定含钙制品中的Ca2 含量,并对微型滴定法与常量滴定法的平行测定结果进行了比较。结果两种方法无显著性差异,F检验t检验结果均在允许范围内,相对偏差均小于2.0%,微型滴定法的精度达到常量滴定法测定水平,能满足化学分析要求。     

铽与苯乙酮酸、2,2''''-联吡啶、1,10-菲口罗啉、三苯基氧膦铽三元配合物的合成、结构表征及荧光性能的研究

以硝酸铽、苯乙酮酸（HL）, 2, 2＇-联吡啶（dipy）、 1, 10-菲啰啉（phen）和三苯基氧膦（TPPO）合成了TbL3dipy（H2O）2, TbL3phen（H2O）2和TbL2（TPPO）2NO3 3种新型固态配合物. 用元素分析、电导率、红外光谱和核磁共振谱对其进行了表征, 确定了配合物的组成. IR表明, 配合物中羧酸根可能以单齿方式配位. 1HNMR显示, 苯乙酮酸根配位后苯环上5个氢原子的化学位移移向高场. 室温下测定了配合物的荧光激发光谱, TbL3dipy（H2O）2, TbL3phen（H2O）2和TbL2（TPPO）2NO3最佳激发波长分别为361.0, 359.0和367.0 nm;分别以最佳激发波长测定了配合物的发射光谱, 配合物TbL3dipy（H2O）2, TbL3phen（H2O）2 和TbL2（TPPO）2NO3显示Tb3＋离子的特征发射光谱, TbL3dipy（H2O）2和TbL3phen（H2O）2均产生四条谱带, 分别归属于^5D4-^7Fj（j= 6, 5,4,3）能级跃迁（TbL3dipy（H2O）2： 489.0, 545.0, 584.0, 620.0 nm;TbL3phen（H2O）2： 490.0, 544.0, 583.0, 620.0 nm）;但在相同测定条件下, TbL2（TPPO）2NO3仅显示5D4-7F5（544.0 nm）能级跃迁光谱. 3种配合物中TbL3dipy（H2O）2发光强度最高.