An Unusual Fullerene–Carbene Adduct: Thermal Motion,Disorder, or Both?**

A single-crystal X-ray study of a fullerene-imidazole adduct at nine temperatures (80 K≤T≤480 K), accompanied by energy calculations, strongly suggested thermal motion of the C₆₀ moiety with respect to the imidazolium heterocycle. Analysis of the anisotropic displacement parameters, calculations of frequencies, and the refinement of disorder models for the crystal at four temperatures (230 K≤T≤380 K) lead to the conclusion that the rotator is moving at all temperatures. The rotation barrier is low, with one preferred crystallographic site and several other energy minima.     

氟化铵快速分解－电感耦合等离子体质谱法测定地球化学样品中的稀土元素

测定地球化学样品中的微量稀土元素常用混酸分解法或碱熔融法,这些常规方法往往存在耗费试剂量多、基体效应大、操作周期长等缺点。本文采用氟化铵作熔剂,在旋盖聚四氟乙烯坩埚中220℃熔融样品,后采用2毫升硝酸和0.5毫升高氯酸、硫酸（1+1）在电热板上继续分解,建立了氟化铵分解 －电感耦合等离子体质谱法测定岩石、土壤和水系沉积物中15种微量稀土元素的分析方法。本方法能快速、有效地分解样品,经三种国家标准物质验证（岩石、土壤、水系沉积物）,方法的准确度ΔlgC在0.001～0.02之间,测定值与认定值相符。方法检出限为0.001～0.04μg／g之间,精密度RSD%在1.11％ ～4.85％之间,能够满足微量稀土元素的分析要求,方法具有简单快捷、消耗试剂少、检出限低、精密度与准确度好等特点,适合于地球化学等地质样品微量稀土元素的批量快速分析测定。     

IR STUDIES OF THE THERMAL DECOMPOSITION OF[Rh_6(CO)_(16) Co_4(CO)_(12)]/SiO_2: EVIDENCE FOR THE FORMATION OF RhCo_3(CO)_(12)/SiO_2

IntroductionThepreparativeapproachofaneffectivebilTldslliccatalystisalwaysasubjectofboortantsignificanceinheterogeneouscatalysis.InourrecentstUdies,wefoundthatthebAnetallitcarbonylclustercoCo3(CO)12favorablygivesthebAnetalliccoCo3clusterontheSiOZsubdueaft…     

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。     

SAPO-34分子筛骨架稳定性的研究

利用差热分析，原位ＸＲＤ技术，高温条件下的焙烧和水蒸气处理并关联其催化性能变化，研究了ＳＡＰＯ－３４分子筛的热及水热稳定性，差热分析结果表明，ＳＡＰＯ－３４的骨架破坏温度高于１３００Ｋ，原位ＸＲＤ跟踪研究证实，ＳＡＰＯ－３４分子筛原粉在高温焙烧以除掉有机胺及随后的降温过程中无明显的骨架破坏；而焙烧型ＳＡＰＯ－３４在空气中放置一定时间后，水分子吸附微孔中明业降低样品的ＸＲＤ峰强度，且降低幅度随放置时     

用草酸胍制备钴酸盐尖晶石

本文采用先驱物法合成钴酸盐尖晶石MCo₂O₄(M=Zn,Ni,Cu,Mg,Cd,Mn)。以草酸胍作为沉淀剂，在溶液中以共沉淀的方法合成草酸盐先驱物。采用热分析(TG和DTA)、化学元素分析、红外光谱等手段对先驱物进行分析表征。通过红外光谱、X射线粉末衍射、扫描电镜对产物进行表征。产物的平均粒度范围在3.5～8.8 μm之间。     

用于昆虫外激素研究的微量顶空收集及热解吸气相色谱进样方法初探

描述了一个结合项空气流收集与无溶剂热解吸气相色谱进样的方法。用填充PorapskQ的微量注射器作为吸附管进行气流收集。将收集物不经溶剂洗脱直接进行热解吸进样。用人工合成的昆虫外激素化合物反-7-十二碳单烯乙酸酯（E-7-DA）及顺-5,反-7-十二碳二烯乙酸酯（Z-5,E-7-DDA）测定了方法的回收率,初步探索了运用于昆虫外激素分析的可行性,并讨论了提高回收率的途径。     

Annealing of melt-crystallized nylon 6

Effect of annealing on thermal behaviour and crystalline structure of meltcrystallized nylon 6 has been investigated.The annealing process is found to be characterized by an incubation period followed by a more or less doubling of the SAXS long spacing and of the crystallinity.The extrapolated heat of melting of the crystalline phase of nylon 6 in the-modification is 188 Jg^–1 and its extrapolated equilibrium melting temperature is 260 °C.Presented in part at 28th IUPAC Symposium on Macromolecules, Strasbourg, July, 1981.     

A computational study of stereospecifity in the thermal elimination reaction of menthyl benzoate in the gas phase

This paper reports a theoretical study, at the B3LYP/6–31 + G(d,p) and M05‐2X/6–31G + (d,p) levels, on the thermal decomposition of menthyl benzoate (2‐isopropyl‐5‐methylcyclohexyl benzoate). It undergoes a unimolecular first‐order elimination to give 3‐menthene (1‐isopropyl‐4‐methylcyclohexene), 2‐menthene (3‐isopropyl‐6‐methylcyclohexene), and benzoic acid. We studied two possible mechanisms trying to explain the formation of 2‐ and 3‐menthene, via six‐membered or four‐membered cyclic transition states. Rate constants were calculated at two temperatures, 587.1 and 598.6 K, and they agree well with the experimentally determined values. We verify that 3‐menthene is the product mainly formed at both temperatures. The progress of the reactions has been followed by means of the Wiberg bond indices. Intrinsic reaction coordinate (IRC) calculations have been carried out to verify that the localized transition state structures connect with the reactants and products and also to verify that the parent compound, menthyl benzoate, is taking the cis‐configuration needed in the reaction. Copyright © 2009 John Wiley & Sons, Ltd.     

Thermal Entanglement of an XY Two-Qutrit Spin Chain with Dzialoshinski-Moriya Interaction

The effect of Dzialoshinski-Moriya （DM） interaction on thermal entanglement of an XY two-qutrit spin chain is investigated. We find that DM interaction and the anisotropy parameter can enhance quantum thermal entanglement to a maximal value individually. However, when both of them take large values, the entanglement is not enhanced, but is destroyed. Our analysis will shed some light on the understanding of the effect of the DM interaction on thermal entanglement of an XY two-qutrit spin chain.