关于meso—四苯基卟啉在冰醋酸中的存在形式

前言卟啉在生物化学、分析化学、药物化学等领域有着广泛研究和重要应用［１～３］。近年来虽然对卟啉类化合物的研究报道很多［４～６］，但对卟啉在酸性介质中的研究很少。较早期的研究工作认为卟啉类化合物在酸性介质中仅以其二酸形式存在［７］。本文实验结果显示ｍｅ...     

A Rapid and Convenient Synthesis of Derivatives of Imidazoles under Microwave Irradiation

An efficient and a quick microwave‐assisted synthesis of benzimidazoles and trisubstituted imidazoles was developed. Three benzimidazoles were obtained as a result of the condensation of 1,2‐phenylenediamine with carboxylic acids and acetoacetic ester without catalyst. A series of trisubstituted imidazoles were synthesized by condensation of benzil, aromatic aldehyde and ammonium acetate in the presence of glacial acetic acid.     

Voltammetry in Undiluted Acetic Acid. In Situ Determination of Water

Water present in undiluted acetic acid can be monitored in situ with Pt and Au microelectrodes using differential pulse and square‐wave voltammetries. Both reduction and oxidation peaks can be obtained. The best quantitative analytical results were obtained for the anodic peak, the Pt microelectrode, and differential pulse voltammetry. The anodic water peak is located at +1.55 V vs. the quasi reference Pt electrode. The voltammetric peak obtained at Pt electrode is apparently not a diffusional one, however, the calibration plot obtained by employing this peak is linear over a wide concentration range, up to 4 mol dm^?3. The detection limit has been estimated as 2.3 mM or 0.0043 v/v%. The developed method may be particularly useful, since the Karl Fischer method can not be used to determine water in glacial acetic acid due to the estrification reaction of acetic acid with methanol. A voltammetric wave of undiluted acetic acid could not be obtained in the positive and negative ranges of potential.     

离子色谱安培检测法测定醋酸中的痕量碘离子

目前较为先进的醋酸生产工艺是甲醇羰基合成工艺,在生产醋酸的过程中加入碘甲烷作助催化剂。然而,碘离子的存在对不锈钢材料具有腐蚀性,所以在合成醋酸的过程中必须严格监测醋酸中碘离子的含量。研究表明[1],测定工业醋酸中痕量碘离子的有效方法是高效阴离子交换色谱(IC)与脉冲     

中国西南山区第四纪冰川堆积物工程地质分类探讨

中国的大陆冰川堆积物几乎都属于巨粒土或块石（漂石）土、碎石土,但因复杂的物质组成和组构特征,各地或同一地区不同成因类型（冰碛、冰水）的堆积物具有极为不同的工程地质性质,其地质体稳定性和地质灾害的易发性存在着显著的差异。我国已有的工程分类框架不能满足当代冰川堆积物甚至其他碎石土（巨粒土）的工程地质和地质灾害研究的需要。中国西南山区冰川堆积物的物质成分、细观结构等的野外调查和室内测试分析结果表明,冰川堆积物的物质成分和组构特征主要表现为：颗粒组成的不均一性和多元性、组构单元的双元性、结构的无序性和胶结性等。冰川堆积物的物质成分和组构特征与其工程性质具有密切的关系,是冰川堆积物工程地质分类的基础。本文探讨了中国西南山区冰川堆积物的工程地质分类问题,提出基于胶结程度和粒度组成的二级分类方案,对冰川堆积物及其他块（漂）石土的工程地质研究和工程实践具有一定指导意义。     

非水滴定法测定二甲基烯丙基胺

研究了在甲胺和二甲胺存在下,以冰乙酸为溶剂,甲酸-乙酸酐为酰化剂,0．1 mol·L-1 高氯酸-冰乙酸标准溶液为滴定剂,10g·L-1结晶紫为指示剂的非水滴定法测定二甲基烯丙基胺 (DMAA)。考察了惰性组分和水分对滴定的影响。结果表明,总胺的测定偏差随着水分的增加而增大;当含水量在5％以内,对二甲基烯丙基胺的测定影响较小,相对误差一般在1％以内,加入约 10％的氯仿可使终点敏锐。与气相色谱法测定结果比较,该法简便,结果准确。     

The Bayesian Change Point and Variable Selection Algorithm: Application to the δ18O Proxy Record of the Plio-Pleistocene

In this article, we introduce the Bayesian change point and variable selection algorithm that uses dynamic programming recursions to draw direct samples from a very high-dimensional space in a computationally efficient manner, and apply this algorithm to a geoscience problem that concerns the Earth's history of glaciation. Strong evidence exists for at least two changes in the behavior of the Earth's glaciers over the last five million years. Around 2.7 Ma, the extent of glacial cover on the Earth increased, but the frequency of glacial melting events remained constant at 41 kyr. A more dramatic change occurred around 1 Ma. For over three decades, the “Mid-Pleistocene Transition” has been described in the geoscience literature not only by a further increase in the magnitude of glacial cover, but also as the dividing point between the 41 kyr and the 100 kyr glacial worlds. Given such striking changes in the glacial record, it is clear that a model whose parameters can change through time is essential for the analysis of these data. The Bayesian change point algorithm provides a probabilistic solution to a data segmentation problem, while the exact Bayesian inference in regression procedure performs variable selection within each regime delineated by the change points. Together, they can model a time series in which the predictor variables as well as the parameters of the model are allowed to change with time. Our algorithm allows one to simultaneously perform variable selection and change point analysis in a computationally efficient manner. Supplementary materials including MATLAB code for the Bayesian change point and variable selection algorithm and the datasets described in this article are available online or by contacting the first author.     

Diastereoselective synthesis of tetrasubstituted-octahydro-3,6-diazacarbazoles and tetrasubstituted-3,6-diazacarbazoles via double Pictet-Spengler reaction

Pictet-Spengler condensation of 2,5-bis(2-phenyl-1-aminoethyl)pyrrole using glacial acetic acid afforded only one diastereomer of unreported tetrasubstituted-octahydro-3,6-diazacarbazoles. These were readily dehydrogenated to tetrasubstituted-3,6-diazacarbazoles. The stereoselectivity in the Pictet-Spengler reaction has been demonstrated using single crystal X-ray analysis.     

四川泸定磨西台地第四纪冰水台地边坡地质灾害易发性研究

河流冲刷对第四纪软弱地层岸坡的地质灾害起到控制性作用。本文以磨西台地冰水堆积物岸坡为例,充分考虑河流与岸坡地质灾害之间的内在联系,基于对实测地质灾害的分析结果,采用Logistic监督分类方法,评价各环境因子（尤其是河流冲蚀特性因子）在河流岸坡稳定性评价中的作用,进而采用高相关的环境因子进行地质灾害易发性预测。研究表明,河流弯曲度、河流流量、岸坡坡度、河床宽度、岸坡宽度与地质灾害的发育相关性强,采用这些参数和Logistic模型预测的地质灾害易发性能很好的反映现状和未来地质灾害的发育特点,进而提出了磨西台地岸坡地质灾害防治的初步建议。