负载铜的活性炭用于低浓度甲硫醇的吸附

采用浸渍法制备了负载铜的木质活性炭样品,研究了负载量、灼烧温度对材料吸附低浓度甲硫醇的性能影响,研究发现负载量和灼烧温度均对材料性能有显著作用,其中最佳的灼烧温度为300℃,最佳负载量为0.7 mmol·g^-1,采用低温氮吸附方法、X射线衍射分析(XRD)、X射线光电子能谱法(XPS)、扫描电子显微镜(SEM)和高分辨透射电镜(HRTEM)等方法对样品进行了表征和分析,从分析结果可知,材料的吸附性能和材料比表面、样品中Cu的价态及分散状况均存在一定关系。经过优化的样品对低浓度甲硫醇表现出了良好的吸附性能,其穿透时间比空白活性炭样品提高6倍以上。     

负载铜的活性炭用于低浓度甲硫醇的吸附

采用浸渍法制备了负载铜的木质活性炭样品,研究了负载量、灼烧温度对材料吸附低浓度甲硫醇的性能影响,研究发现负载量和灼烧温度均对材料性能有显著作用,其中最佳的灼烧温度为300℃,最佳负载量为0.7 mmol·g~(-1),采用低温氮吸附方法、X射线衍射分析(XRD)、X射线光电子能谱法(XPS)、扫描电子显微镜(SEM)和高分辨透射电镜(HRTEM)等方法对样品进行了表征和分析,从分析结果可知,材料的吸附性能和材料比表面、样品中Cu的价态及分散状况均存在一定关系。经过优化的样品对低浓度甲硫醇表现出了良好的吸附性能,其穿透时间比空白活性炭样品提高6倍以上。     

甲烷水合物在静态体系中生成反应的促进

静态体系生成甲烷水合物是个缓慢的、不完全的过程。即使使用表面活性剂也不能实现反应物的100％转化。本文讨论了在静态反应停止后,使用系统温度振荡的方法来促进水合反应的继续进行,直至完全转化。在系统温度从-10～4℃之间周期振荡时,原本停滞的水合反应在水的相变温度附近又开始发生反应,由于水合物合成时铠甲效应的存在,水在样品中的过冷度达到10℃左右。文中对样品的热物性测试表明,在经过几个温度变化周期后,反应非常完全,反应器中样品是100％的甲烷水合物。     

顶空-气相色谱法测定水中三氯甲烷和四氯化碳方法的改进

改进了顶空-气相色谱法测定水中三氯甲烷和四氯化碳的方法,对平衡温度和平衡时间进行了优化,对不同溶剂配制的标准使用液和不同方法制作的工作曲线对测定结果的影响进行了比较.试验结果表明,样品最佳平衡温度和时间分别为50℃和35 min.采用甲醇代替标准中规定的纯水配制标准使用液,采用微量进样针取样到预先密封的顶空瓶中,三氯甲...     

拉伸对聚左旋乳酸结晶的影响

在成型加工过程中,拉伸是提高聚合物材料结晶能力的一种重要手段. 本文采用红外光谱、差示扫描量热分析、X射线衍射等方法系统研究了不同温度下拉伸对聚左旋乳酸（PLLA）结晶行为的影响. 结果表明,在合适的温度条件下,拉伸能迅速提高PLLA的结晶速度和结晶度. 对经过拉伸预处理但未结晶的PLLA样品进行等温及非等温结晶的研究发现,经过拉伸预处理的PLLA样品的结晶速率和结晶度都得到提高,这表明预拉伸会影响PLLA在后续过程中的结晶行为.     

极谱法测定地质样品中锡的方法改进

过氧化钠熔融分解样品,热水浸提,试样经铍盐做共沉淀剂,用乙二胺四乙酸(EDTA)消除钙、镁等的影响,在盐酸-氯化铵底液中,用极谱法对锡进行测定,改进并简化了国标方法.对极谱法测定地质样品中锡从熔矿方式、测试温度以及干扰元素的影响及消除等方面进行探讨,并对仪器的工作条件进行优化.锡的方法检出限为10.0μg/g.方法经标准物质验证,测定值与标准值相吻合,并进行不同仪器和方法的对比实验,结果一致,准确度高.方法精密度(RSD,n=12)低于2%.方法效率高、测定结果准确可靠,已应用于大量地质样品的分析中.     

湿法消解–石墨炉原子吸收标准加入法测定土壤中的镉

土壤样品经过硝酸–氢氟酸于130℃加热回流处理后,采用石墨炉原子吸收标准加入法测定半消解样品中镉的含量。以5%氯化铵或0.1%硝酸钯作为化学改进剂,灰化温度为500℃、原子化温度为2 000℃。当标准系列吸光度在0.18以内时,镉标准溶液的质量浓度在0~3.0μg/L内与吸光度呈良好的线性,相关系数r=0.998 6,方法的检出限为0.02 mg/kg,实际样品测定结果的相对标准偏差为3.93%~5.30%(n=5)。用该法与国标方法对土壤标准样品进行测定,两种方法测定结果一致。该法快速、简便,适用于土壤中镉含量的快速检测。     

浮游植物体内叶绿素a测定方法的改进

对丙酮萃取分光光度法测定浮游植物体内叶绿素a的方法进行改革。改进法在样品经过冷冻、50℃热丙酮快速提取并放置2h后后进行测定。对改进前后方法测定结果的方法分析表明，方法改进前后测定结果不存在显著性差异。方法改进后简化了操作，提取时间由原来的8-20h缩短为1.5-2.5h。     

DSC法测定PS玻璃化温度的再研究

对Fevotte提出的由DSC曲线构建玻璃化温度谱图的方法进行了改进,将橡胶态含量为0.5时的温度定义为聚合物的Tghr.采用改进Fevotte方法重新研究了PS的玻璃-橡胶态转变,PS的Tghr值比半比热外推法结果Tghc高约4K,当考察热处理时间和降温速率对聚合物玻璃-橡胶态转变的影响规律时,改进方法得到的结果与理论分析更为一致.聚合物的Tghr受热历史影响,随热处理条件改变,通过对不同降温速率冷却后样品滞后焓数据的拟合,推测PS样品的Tghr在377.5～390.9K范围内变化.     

高效液相色谱-荧光检测法测定环境样品中的过氧化物

对高效液相色谱-荧光检测法测定过氧化氢和有机过氧化物的方法进行了改进,从而提高了方法的检测灵敏度。以氯化血红素(hemin)作催化剂进行柱后衍生反应,过氧化物将对羟基苯乙酸氧化生成能吸收荧光的二聚物,然后用荧光检测器检测。实验确定了最佳反应管温度和荧光检测波长。应用该法测定了大气和雨水样品中过氧化物的浓度。     

α-Amino acid derived enaminones and their application in the synthesis of N-protected methyl 5-substituted-4-hydroxypyrrole-3-carboxylates and other heterocycles

A new and simple synthesis of novel N-protected methyl 5-substituted-4-hydroxypyrrole-3-carboxylates, which exist in equilibrium with their 4-oxo tautomers, has been developed in two steps starting from N-protected α-amino acids. The key intermediates are enaminones, which can also be isolated, characterized, and used for the construction of other functionalized heterocycles, before they spontaneously decompose to pyrrole products. 4-Hydroxypyrroles are prone to partial aerial oxidation but can be efficiently alkylated or reduced to stable polysubstituted pyrrolidine derivatives.     

Specific intramolecular aromatic CH insertion of diazosulfonamides

The chemoselectivity in the intramolecular CH insertion of various diazosulfonamides has been experimentally studied. The results reveal that the aliphatic 1,4-, 1,5-, or 1,6-C(sp³)?H insertions of diazosulfonamides are not accessible, while the aromatic 1,5-C(sp²)?H insertion can be realized specifically by adjusting the diazo-adjacent group. In addition, the general chemoselectivities in the intramolecular CH insertions of diazosulfonyl compounds are summarized. Generally, diazosulfones undergo both aromatic 1,5-C(sp²)?H and aliphatic 1,5- and 1,6-C(sp³)?H insertions, while diazosulfonates undergo aliphatic 1,5- and 1,6-C(sp³)?H insertions. However, diazosulfonamides only undergo aromatic 1,5-C(sp²)?H insertion.     

N-Heterocyclic carbene-palladacyclic complexes: synthesis,characterization and their applications in the C-N coupling and α-arylation of ketones using aryl chlorides

N-Heterocyclic carbene-palladacyclic complexes 3 were successfully achieved in a one-pot procedure under mild conditions. The structure of 3a was unambiguously confirmed by X-ray single crystal diffraction and it was an active catalyst in the Buchwald-Hartwig amination and α-arylation of ketones even at very low catalyst loadings (0.01?mol%).     

Iodine-mediated oxidative Pictet-Spengler reaction using terminal alkyne as the 2-oxoaldehyde surrogate for the synthesis of 1-aroyl-β-carbolines and fused-nitrogen heterocycles

An efficient iodine-mediated oxidative Pictet-Spengler reaction in dimethyl sulphoxide (DMSO) using terminal alkynes as the 2-oxoaldehyde surrogate for the synthesis of aryl (9H-pyrido[3,4-b]indol-1-yl)methanones is described. The scope of the protocol includes the total synthesis of Fascaplysin, Eudistomins Y₁ and Y₂. The methodology is extended for preparing pyrrolo[1,2-a]-quinoxaline and indolo[1,5-a]quinoxaline derivatives. The utility of 1-aroyl-β-carbolines was demonstrated by performing palladium-catalyzed β-carboline directed ortho-C(sp2)-H functionalization of the phenyl ring with thiomethyl (SMe) group using DMSO as source and for accessing 4-aryl-canthin-6-ones.     

Facile synthesis of bicyclic 1-arylpyrazol-5-ones

In this Letter, we described a facile method for constructing fused bicyclic 1-arylpyrazol-5-one ring system. We employed various methylene-containing carboxylic acids as the substrates and proved that the pyrazolone ring closure requires activated methylene group in intermediate II. Accordingly, a series of structurally diversified, fused bicyclic 1-arylpyrazol-5-ones was prepared in moderate to high yields using the requisite substrates.     

Synthesis of pyrrolo[1,2-a]pyrazines and pyrazino[1,2-a]indoles by Curtius reaction in Morita-Baylis-Hillman derivatives

Synthesis of substituted pyrrolo[1,2-a]pyrazines and pyrazino[1,2-a]indoles from the Morita-Baylis-Hillman derivatives of acrylates via saponification followed by Curtius reaction is described.     

正丁胺对激光染料荧光谱影响的研究

用正丁胺作为碳源,采用射频辉光放电制备碳膜,选用激光染料R6G和聚乙二醇混合液作为蒸气源,采用单源热蒸发,在蒸发室与染料同时沉积得到混合膜,用拉曼光谱和红外光谱分析了碳膜的结构和键合方式,分析表明:碳膜中存在胺基团和氢原子.混合膜的荧光谱测量结果表明,认为正丁胺对染料荧光谱的影响是因为胺基和氢原子的存在.     

Cu0-catalysed 1,3-dipolar cycloadditions of α-amino acid derived N,N-cyclic azomethine imines to ynones

A series of 20 CuAIAC reactions between eight 4-acylamino substituted pyrazolidine-3-one-1-azomethine imines and four terminal ynones were performed using Cu⁰ as catalyst. The corresponding fluorescent cycloadducts were obtained in very high yields upon simple workup. Thus, Cu-metal turned out to be a better catalyst than Cu^I in terms of yield and ease of isolation. Availability of azomethine imines, mild reaction conditions, and simple workup enable a “click” access to libraries of densely substituted 2,3-dihydro-1H,5H-pyrazolo[1,2-a]pyrazol-1-ones. Reactivity of differently substituted dipoles was evaluated experimentally and by quantum chemical methods (DFT).     

Synthesis and antioxidative/anti-inflammatory activity of novel fullerene–polyamine conjugates

(E)-4-(Fullerenopyrrolidin-1-yl)-3-methylbut-2-enoic acid and its corresponding succinimidyl ester, readily obtained through Prato-type modification of C₆₀, were used for the selective N-acylation of polyamines. The thus obtained conjugates were evaluated for their antioxidative and anti-inflammatory activity and their cytotoxicity was determined. Members of this family of compounds showed interesting anti-lipid peroxidation, anti-lipoxygenase and anti-inflammatory activity and comparable cytocompatibility to spermidine.