壳聚糖对Cd2+的吸附性能

壳聚糖(ｃｈｉｔｏｓａｎ,简称ＣＴＳ)是由虾、蟹壳脱钙、蛋白质和脂肪后、经化学改性得到的天然高分子聚合物,分子中存在能与金属离子配位的羟基或氨基,其配合物可作为絮凝剂和螯合吸附剂用于水处理[1 3]及湿法冶金[4]等。本文考察了壳聚糖对Ｃｄ2+的静态吸附性能。1　实验部分1.1　试剂与仪器壳聚糖(浙江玉环县化工厂);硫酸镉、硝酸镉(分析纯,广州化学试剂厂);碳酸镉(化学纯,上海试剂二厂),其余试剂均为分析纯。78 1型磁力加热搅拌器(江苏金坛市恒丰仪器厂),501型超级恒温器(上海实验仪器厂),ｐＨＳ 3型酸度计(上海第二分析仪器厂)。1…     

DL-蛋氨酸铋(Ⅲ)固体配合物的合成、表征和XRD数据指标化

许多氨基酸的金属配合物具有抗菌、抗炎、抗癌和拮抗作用等生物活性[1,2 ] 。铋的化合物在医药中也有着广泛的应用 ,如柠檬酸铋用于治疗胃病[3 ] ,某些铋的化合物也用于外科处理创伤和止血 ,为了寻找副作用小、疗效更好的抗溃疡新药 ,我们通过固 固反应合成了ＤＬ 蛋氨酸合铋 (Ⅲ )配合物。利用固相反应合成生物无机配合物 ,可有效地避免某些金属盐的水解 ,具有操作简单、副反应少、产率高等特点[4,5] 。1　实验部分1 1　主要仪器与试剂85 2型恒温磁力搅拌器 (上海司乐仪器厂 ) ,ＤＧＦ30型电热恒温干燥箱 (南京实验仪器厂 ) ,Ｄ2 60型恒…     

四苯骈卟啉金属配合物轴向配位反应的热力学性质研究

金属卟啉在生命过程中起着重要的作用[1 - 4 ] 。CuTBP ,CoTBP与有机碱的反应,用光度法测定了轴配反应在不同温度下的速率常数和平衡常数,求得活化能及热力学参数,结果表明:它们与不同有机碱反应的活化能及平衡常数既与配体的碱性有关,也与空间位阻有关,同一温度下反应的平衡常数和速率常数的大小顺序均为:咪唑>吡啶>2 甲基吡啶>2 ,4 二甲基吡啶。1　实验部分1 .1　仪器与试剂日本产岛津UV 2 4 0G型分光光度计,上海分析仪器厂72 1型光度计(内装恒温套) ,重庆电机厂超级恒温槽。四苯骈卟啉金属配合物系自制[4] ,咪唑、吡啶、2 甲基吡…     

在硝酸钠存在下硫氰酸铵-孔雀绿-水液-固体系浮选分离锌(Ⅱ)的研究

在硝酸钠存在下硫氰酸铵 -孔雀绿 -液 -固体系能够浮选分离锌 (Ⅱ ) ,结果满意。与文献[2～ 6] 相比 ,试剂用量更少 ,更为经济 ;与有机溶剂萃取浮选及泡沫浮选分离相比 ,既不使用有害的有机溶剂 ,又不需要复杂的仪器设备 ,因而具有一定的应用和研究前景。1　实验部分1 1　主要试剂与仪器1 .0× 1 0 -3ｍｏｌ Ｌ孔雀绿 (ＭＧ)水溶液 ;0 .1ｍｏｌ ＬＮＨ4 ＳＣＮ溶液 ;硝酸钠、溴化钾、氯化钠、硫酸铵及所用其它试剂均为分析纯。72 1型分光光度计 (上海第三分析仪器厂 ) ;ｐＨＳ 2酸度计 (上海第二分析仪器厂 )。1 2　实验方法于 2 5ｍｌ磨…     

氧化苯胺蓝褪色光度法测定微量铬

铬是生物体所必需的微量元素 ,也是主要环境污染物质之一 ,是控制环境污染的一项重要指标 [1]。铬的工业来源主要是含铬矿石的加工、金属表面处理、皮革制鞋、印染等行业。铬的测定可采用二苯碳酰二肼法、原子吸收光谱法等 [2 ]。本文建立了 Cr( )氧化苯胺蓝褪色来测定铬的方法。实验表明 ,在 H2 SO4 介质中 ,Cr( )氧化苯胺蓝褪色的程度与 Cr( )的含量呈线性关系。方法已用于土壤及淤泥中微量铬的测定。1　实验部分1 .1　仪器和试剂72 1型分光光度计 (上海第三分析仪器厂 )。苯胺蓝溶液 :0 .2 g/L;铬标准溶液 :称取 0 .2 82 9g干燥过…     

茜素黄R-OP体系测定铁的研究

茜素黄 R是一种指示剂 ,已用于镁 [1]、钛 [2 ]和铁 [3]的分析 ,文献 [3]应用了阳离子表面活性剂CTMAB作增敏试剂。本文探讨了以非离子表面活性剂 OP作增敏试剂测定铁 ,结果表明 ,在 OP存在下 Fe3 与茜素黄 R在 p H8.2～ 9.5内形成组成比为 1∶ 3的配合物 ,铁量在 0～ 40 μg/2 5ml内服从比耳定律 ,在此基础上拟定了分析方法 ,用于磷矿样中铁的测定 ,结果与邻菲罗啉法一致。1　试验部分1 .1　主要仪器与试剂72 1型分光光度计 (上海第三分析仪器厂 )UV- 754型分光光度计 (上海第三分析仪器厂 )Fe( )标准溶液 :1 0 0μg· ml-1,称取分…     

火焰原子吸收光谱法间接测定食品中碘

微量碘的测定一般采用光度法。本文依据 [Ｃｄ(Ｐｈｅｎ) 3]2 + 与Ｉ- 可形成 [Ｃｄ(Ｐｈｅｎ) 3]2 + (Ｉ- ) 2 离子对的原理[1] ,用硝基苯萃取 ,通过测定有机相中镉的含量 ,间接测定碘。用于测定含碘食品 ,结果满意。1　试验部分1.1　主要仪器与试剂ＷＦＸ 1Ｂ型原子吸收分光光度计 (北京第二光学仪器厂 )ｐＨＳ Ⅰ型酸度计 (上海分析仪器厂 )涡流混合器 (上海第一医学院仪器厂 )碘标准储备液 :10ｍｇ·ｍｌ- 1,准确称取碘化钾(ＧＲ) 13.0 80 0ｇ ,用少量无碘水溶解后 ,定容于 1Ｌ容量瓶中。碘标准使用液为 1ｍｇ·Ｌ- 1。三邻菲罗啉镉溶液…     

萃取色谱—吸光光度法检测镍中微量钴

钴是镍中最常见杂质,光度法分析镍中钴时要求Co:Ni≥1:60,否则镍对分析有较大干扰.文献[4]采用镁型P507树脂分离钴、镍,EDTA滴定法可用于混合液中常量镍的分析.本文研究采用萃取色谱法富集、亚硝基R盐吸光光度法分析镍中微量钴.1 试验部分1.1 主要仪器与试剂721分光光度计(上海第三分析仪器厂)硬质玻璃色谱柱((?)9mm)IL-951原子吸收光谱仪(美国实验仪器公司)pHS-3型精密酸度计(上海第二分析仪器厂)WLB-80型电子微量泵(浙江新昌国康仪器厂)P507萃淋树脂(江苏如东化工厂,萃取剂含量55%)     

硫酸锌与L-α-色氨酸配合行为的相化学研究

锌是重要的生命元素 ,L- α-氨基酸是人体蛋白质的基本结构单元。 α-氨基酸锌配合物作为添加剂在药物、食品和化妆品中有广阔的应用前景 [1～ 3 ] 。本文用半微量相平衡方法 [4] 研究了Zn SO4- Try- H2 O体系在 2 5℃的相化学 ,发现该体系中未形成新化合物。合成了未见文献报道的 Zn( Try) 2 固态配合物 ,并研究了它的物理化学性质。1　实验部分1 .1　仪器与试剂恒温槽 (自制 )温度涨落± 0 .0 5℃ ;WZS— 1型阿贝折光仪 (上海实验仪器厂 ) ;ZD— 2型自动电位滴定仪 ;BRUKER EQ UINOX— 550型傅立叶红外分光光度计 ( KBr压片 )…     

4,11,18,25-四(2-羧基苯偶氮)-1,8-15,22-四己基杯[4]间苯-3,5,10,12,17,19,24,26-八酚的合成及其与钴Ⅱ的显色反应

1　引　　言偶氮类试剂由于其性质稳定、显色反应灵敏度高而被广泛应用 ,为了进一步提高其反应的选择性 ,人们作过很多有效的努力 ,如建立独特的反应条件或反应体系 ,改造试剂的分子结构等。拟通过给偶氮类试剂引入一个环状的刚性环(外向式杯 [4 ]芳烃 )来提高其反应的选择性 ,结果令人满意。2　实验部分2 1　主要仪器与试剂　 72 1型分光光度计 (厦门分析仪器厂 ) ;ＵＶ 2 6 0可见 紫外分光光度计 (日本岛津公司 ) ;ＰＨＳ 3Ｃ型数字酸度剂 (上海雷磁仪器厂 ) ;Ｉｍｐａｃｔ 410型红外光谱仪 (美国尼高力公司 )。间苯二酚、正庚醛、对氨…     

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.