Maleinsäure- und fumarsäureester als liganden in metallcarbonyl-komplexen: I..Mehrkernige molybd;iN'tricarbonyl-ko.niplexe mit 7jr koordinierte-n mxleinsaure- und fumarsaureesterin

Reactions of cycloheptatrienemolyhdenum tricarbonyl. CH,1kNlO(CO)3,with a number of maleic acid or fumaric acid esters (L) at 60-80'C do not give the expected monoculear tricarbonyl derivatives i%10(CO)3L3 but yield binuclear CO-bridge complexes in which the ester molecules are -,coordinated across the t C=C double bond: 60-80'c 2 C7Hs.%lo(CO)3 + 4 L cvc1ohenane , UNIO(CO)3L,12 + 2 C,7Ha At 100'C a polymetric complex with the composition [ MO(CO)3(D1NT FU)Z I,which is also CO-bridged, is obtained with dirnethyl furnarate (DM FU).This compound exists in a tenperature-dependent equilibrium with the binuclear isomer: UNIO(CO)ADNIFU)212 100'C. cN clohe I? jN1o(CO)j(D1N1FU):! L 2WC. benzene X (yellow) (red) The structure have been confirmed on the basis of molecular weight determinations,IR,Raman, 'H N-NMR, ! 3 C NINIR, and UV spectra- The carbonyl stretching force contstants for the binuclear complexes have been calculated using the Cotton-Kraihanzel method and the CO-MO-CO angles have been estimated.     

The electron microscope characterization of the fine structure of nylon 6: I. The supermolecular structure in melt-cast,isotropic bulk material

The application of phosphotungstic acid (PTA) as a staining agent with appropriate hardening procedures and accurate ultra-thin sectioning has enabled the direct transmission electron microscope (TEM) investigation to be carried out on the lamellar fine structure of bulk nylon 6. Details of the organization of the crystal lamellae within spherulites and other morphological structures, their shape and, especially, their dimensions were revealed and the mean structural long period was determined. Interspherulitic regions without any indication of crystalline ordering could be observed in samples which were rapidly cooled from the melt. The investigations on bulk material were completed by observations on solution-grown thin films. Optical diffraction (OD) was used for evaluating the electron micrographs; the results were compared with the data from small angle X-ray scattering (SAXS).     

铸造铝青铜合金Cu-14Al-4Fe-Mn的摩擦磨损性能

用往复式摩擦磨损试验机考察了新型高强度、高耐磨性铸造铝青铜合金Cu-14Al-4Fe-Mn(代号HSWAB)的摩擦磨损性能,利用形貌扫描电子显微镜观察分析了合金磨损表面形貌,探讨了其磨损机理.结果表明,HSWAB合金在干摩擦和油润滑条件下的摩擦磨损性能及磨损机理存在明显差异.在干摩擦条件下,合金中脱落的硬质点及氧化物等磨粒导致较为严重的磨粒磨损,摩擦系数高、磨损率大,主要磨损机理为磨粒磨损、粘着磨损、氧化磨损及疲劳磨损.在油润滑条件下,摩擦系数和磨损率均显著降低,疲劳磨损和氧化磨损受到抑制,主要磨损机理为磨粒磨损和粘着磨损.Cu-14Al-4Fe-Mn合金在油润滑条件下的摩擦系数低达0.08,磨损率低达3.7×10-6g/m,是一种优良的耐磨材料.     

铁基大块非晶合金的摩擦磨损性能研究

采用电弧熔炼、铜模吸铸法制备Fe基大块非晶合金,利用球-盘式摩擦磨损试验机进行干摩擦磨损试验,研究了铸态Fe基大块非晶合金的摩擦磨损行为及热处理对其耐磨性的影响,利用扫描电子显微镜观察合金磨损表面形貌,分析了Fe基大块非晶合金以及相同成分晶态合金的磨损机理.结果表明:在本试验条件下,铸态Fe基大块非晶合金的耐磨性高于相同成分的晶态合金,热处理可以有效提高铸态Fe基大块非晶合金的耐磨性,在保持完全非晶状态的前提下,退火态非晶合金的磨损率较铸态非晶合金减小约40%;材料的结构和性能对合金的摩擦系数影响不大,当进入稳定阶段后Fe基大块非晶合金的摩擦系数稳定在0.58左右;不同处理状态的Fe基大块非晶合金和相同成分晶态合金的磨损机制不同,非晶合金的磨损机制以疲劳磨损为主兼有磨粒磨损,相同成分晶态合金的磨损机制为粘着磨损和磨粒磨损共同作用的结果.     

乙酸铵离心交换法和乙酸钙离心交换法测定土壤阳离子交换量

土壤阳离子交换量(CEC)的测定在农业中有重要的意义,对农业行业标准NY/T295—1995和NY/T1121.5—2006中的离心交换法测定土壤中CEC值的方法进行了优化,讨论了不同pH值的土壤样品对两种方法的选择依据,分析了CEC值测定重现性较差的原因。结果表明,pH值的范围是方法选择的重要依据,pH7.0的样品适合用乙酸铵离心交换法,pH≥7.0的样品则适用乙酸钙离心交换法。优化后方法的准确度和精密度有了较大的改善,实验中对各步骤的优化缩短了约40%的操作时间,减少工作量,适合于批量样品的准确测定。     

Synthesis of an ansa-Zirconocene via a Novel S4-Symmetric Spirobis(silastannaindacene) Compound

A stereoselective reaction of Sn(NMe ₂ ) ₄ with the silyl-bridged bis(cyclopentadienyl) derivative 1 generates the novel spiro compound 2 , in which two C₂-symmetric six-membered rings of opposite configuration are joined at a tin center: One ring is R,R-, and the other S,S-configured. Subsequent reaction with two equivalents of ZrCl₄ affords, by stereoselective Sn/Zr exchange, exclusively the C₂-symmetric isomer of the ansa-zirconocene rac- 3 .     

纳氏试剂测定水中氨氮影响因素的探讨

对国家生活饮用水标准检验方法"GB/T5750—2006"中涉及到的水中氨氮的检测条件进行了探讨,讨论了样品的采集与保存,影响显色、空白值的各项因素,并提出相应的解决办法。对国家标准物质以及实际样品的验证表明,方法的相对误差为0.03%~1.5%,相对标准偏差RSD为0.55%~5.3%,准确度也能满足分析要求,对国家标准方法进行了补充与细化,在实际工作中有参考价值。     

干空气和冷冻水联产除湿空调节能特性研究

本文提出了一种将转轮除湿和再生式蒸发冷却相结合来实现干空气和冷冻水联产的除湿空调系统,以各组成部件为基础,建立了该系统的计算模型,并对其节能特性进行了分析.结果表明,ARI夏季工况下,干空气和冷冻水联产空调的热力COP在1左右,电力COP可达9.03,相应电力消耗和CO2排量比常规空调减少72.69%之多.存在使系统具有较好性能结构的再生温度范围.可以通过改变干空气比来调节潜/显热处理能力,进而实现无能量浪费地提供全部所需冷量.     

Unsymmetrically substituted triazacyclohexanes and their chromium complexes

The unsymmetrically N-substituted N,N′-Ar₂-N″-R-1,3,5-triazacyclohexanes 1–4 (Ar = ortho- or para-fluorophenyl, R = n- or iso-propyl) can be obtained in good yields from a one-step condensation reaction with excess amine. Solid state structures of 1–4 resemble closely those of their triaryl-substituted analogues. The condensation reaction to 4 was looked at by detailed NMR investigations and revealed that amine/aniline exchange is occurring in solutions containing free aniline even at ambient conditions setting up an equilibrium between all possible symmetrical and unsymmetrical triazacylcohexanes. Selective crystallisation of 4 from the solution drives the reaction to high yields of 4. Complexes 1–4 react readily with CrCl₃ or CrCl₃(THF)₃ to form the corresponding CrCl₃ complexes. The complexes are insoluble in non-polar solvents and decompose under decomplexation in coordinating solvents.