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…     

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…     

掺杂合成纳米WO3

掺杂SiO2的WO3粉体对NOX、NH3等多种气体十分敏感,可用于某些特定场合和环境监测方面[1,2]。本文以钨酸铵和硅酸乙酯为原料,分别采用固相法和沉淀法制备了不同掺杂量的SiO2 WO3纳米粉体,并对其进行了XRD,TEM表征。1　实验部分1 1　仪器与试剂德国布鲁克D8X 射线衍射仪;日本电子公司JEM 100SX型透射电子显微镜;天津卫东电炉厂RJX 5 13型马弗炉;上海司乐仪器厂85-2型恒温磁力搅拌器。钨酸铵(NH4)5H5[H2(WO4)6]H2O(化学纯);硅酸乙酯(C2H5O)4Si(分析纯);无水乙醇CH3CH2OH(分析纯);盐酸HCl(分析纯)。1 2　固相法制备WO3…     

反相高效液相色谱法测定微乳制剂中的胰岛素

Waters高效液相色谱仪：510型泵,486型紫外检测器．WDL-95色谱工作站(大连化学物理研究所);PHS-3C型精密pH计(上海雷磁仪器厂);SB2200型超声仪(上海必能信超声有限公司)。猪胰岛素(26．8IU／mg,徐州生化厂);乙腈(色谱纯,Fisher公司);Triton X-100(分析纯,Amresco公司);其余试剂均为国产分析纯,水为双蒸水;胰岛素微乳制剂及辅料(本校生命科学与技术学院药物研究所)。     

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…     

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…     

铝在氢氧化钠溶液中的电化学行为研究

铝是地壳中含量丰富的元素 ,分布广泛 ,由于其具有价格低、能量密度高、导电性良好及无毒性等优点 ,因而是阳极材料的首选物质 ,铝电池的研究也已经成为近年来研究开发的热点课题之一[1～ 3] 。探讨铝在强碱性溶液中的溶解机理 ,对铝电池的研究和开发将具有一定的理论指导意义。1　实验部分1 1　仪器与试剂ＢＡＳ 1 0 0Ａ电化学系统 (美国ＢＡＳ仪器公司 ) ;ＣＳ5 0 1型恒温槽 ;工作电极为直径是 0 .3ｍｍ的铂圆盘电极 ,参比电极是标准甘汞电极 (ＳＣＥ)。铝( 99.99% ) (天津化学试剂厂 ) ,氢氧化钠为分析纯(上海化学试剂厂 ) ,水为二次蒸…     

3,3′-二磺酸基联苯氨基重氮偶氮苯与镍的显色反应及其分析应用

1　引　　言镍是制作催化剂和纳米材料的重要物质 ,也是生物与人体中重要的微量元素。三氮烯类显色剂作为测定镉、汞、镍等的高灵敏试剂研究得比较多。但用双三氮烯测镍的研究未见报道。我们用自己合成的双三氮烯 3,3′ 二磺酸基联苯氨基重氮偶氮苯 (ＤＳＤＰＡＤＡ)与镍的显色反应 ,结合萃取分离用于人发、大米、油菜中痕量镍的测定 ,结果满意。2　实验部分2 .1　仪器与试剂　ＵＶ 2 6 0型分光光度计 (日本岛津公司 ) ;72 2型光栅分光光度计 (上海第三分析仪器厂 ) ;ＰＨＳ 3Ｃ酸度计 (上海雷磁分析仪器厂 )。镍标准溶液 :准确称取纯金属镍…     

毛细管气相色谱法测定室内空气中苯含量

苯已被国际癌症研究中心(IARC)确认为致癌物质[1],一般是通过吸入蒸气或皮肤吸收而使人中毒。装修中苯作为溶剂、粘合剂、添加剂被广泛用于涂料、板材,以蒸气状态存在于空气中[2]。本文对毛细管气相色谱法测定室内空气中苯的适宜条件进行了探讨,经实际样品测定,结果令人满意。1　实验部分1.1　仪器与试剂　　岛津GC 9A气相色谱仪,氢火焰离子化检测器(FID),C R6A处理机;KJ 201型振荡器;5 0μL进样器。二硫化碳为分析纯(上海试四赫维化工有限公司),净化后取1 0μL注入色谱仪应无杂峰出现[3];苯为色谱纯(上海试剂一厂)。1.2　标准储…     

苯偶氮水杨醛异烟酰腙与镉的高灵敏度荧光反应及其应用

1引言镉是一种剧毒重金属。长期接触镉,能引起多种癌症。人们急需各种改进的方法来检测各种环境样品、工业废水以及生物组织里的Cd2 含量。本研究合成了新荧光试剂苯偶氮水杨醛异烟酰腙(BSIH),实验了试剂与镉的荧光反应新体系的最适宜条件。建立了一个新的测定痕量镉的荧光分析方法,方法的线性范围为0.6~120.0μg/L;检出限为0.32μg/L,方法成功地应用于自来水、河水和废水中镉的测定。2实验部分2.1仪器与试剂RF-5000型荧光光度计(日本岛津公司);PHS-2C型pH计(上海雷磁仪器厂);Cd2 标准溶液1 g/L;标准工作液:1μg/L;1×10-4mol/L苯偶…     

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.