双水相萃取法分离铍(Ⅱ)、铁(Ⅲ)与铁(Ⅱ)、铬(Ⅲ)、锰(Ⅱ)、铝(Ⅲ)

研究了在聚乙二醇2000(PEG)-硫酸钠(Na2SO4)-邻苯二酚紫(PV)体系中铍(Ⅱ)、铁(Ⅲ)、铁(Ⅱ)、铝(Ⅲ)、铬(Ⅲ)、锰(Ⅱ)的萃取行为。试验结果表明,铍(Ⅱ)在pH 3.5-7.0及铁(Ⅲ)在pH 4.0-7.0范围内可以被PEG相几乎完全萃取,而铝(Ⅲ)、铬(Ⅲ)在pH 1.0-7.0、锰(Ⅱ)在pH 1.0-4.5、铁(Ⅱ)在pH 1.0-4.5则不被萃取。从而实现了将铍(Ⅱ)(pH 3.5)、铁(Ⅲ)(pH 5.0)与铝(Ⅲ)、铬(Ⅲ)、锰(Ⅱ)、铁(Ⅱ)混合离子的定量分离。同时探讨了PEG相的萃取机理。     

硫酸铵-锌试剂-Tween 80体系萃取分离铜(Ⅱ)、钴(Ⅱ)、镍(Ⅱ)、锌(Ⅱ)、镉(Ⅱ)、锰(Ⅱ)

研究了(H4)2SO4-Zincon(锌试剂)-Tween 80体系萃取分离金属离子Cu(Ⅱ)、Co(Ⅱ)、Ni(Ⅱ)、Zn(Ⅱ)、Cd(Ⅱ)、Mn(Ⅱ)的行为.试验表明,Cu(Ⅱ)、Co(Ⅱ)、Ni(Ⅱ)在pH 6～9范围内,与Zincon形成的螯合物可被Tween 80相完全萃取,而Zn(Ⅱ)、Cd(Ⅱ)、Mn(Ⅱ)基本不被萃取,进而实现了Cu(Ⅱ)、Co(Ⅱ)、Ni(Ⅱ)与Zn(Ⅱ)、Cd(Ⅱ)、Mn(Ⅱ)混合离子的定量萃取分离.     

用聚乙二醇-硫酸铵-铝试剂体系萃取分离铁(Ⅲ)、铝(Ⅲ)、铜(Ⅱ)、钴(Ⅱ)、镉(Ⅱ)、锰(Ⅱ)、镍(Ⅱ)

研究了在聚乙二醇-硫酸铵-铝试剂体系中Fe（Ⅲ）、Al（Ⅲ）、Cu（Ⅱ）、Co（Ⅱ）、Cd（Ⅱ）、Mn（Ⅱ）、Ni（Ⅱ）的萃取分离行为．结果表明，在pH 5．0～6．5HAc-NaAc 缓冲溶液中，Fe（Ⅲ）、Al（Ⅲ）可被 PEG相几乎完全萃取，而 Cu（Ⅱ）、Co（Ⅱ）、Cd（Ⅱ）、Mn（Ⅱ）基本上不被萃取，从而实现了 Fe（Ⅲ）与 Cu（Ⅱ）、Co（Ⅱ）、Cd（Ⅱ）、Mn（Ⅱ）及Al（Ⅲ）与 Fe（Ⅲ）、Co（Ⅱ）、Cu（Ⅱ）混合离子的定量萃取分离。井研究了不同类型的表面活性剂对PEG相萃取行为的影响。     

硫酸铵-锌试剂-Tween-80体系萃取分离铜(Ⅱ)、钴(Ⅱ)、镍(Ⅱ)、锌(Ⅱ)、镉(Ⅱ)、锰(Ⅱ)

研究了（NH4）2SO4－Zincon（锌试剂）－Tween-80体系萃取分离金属离子Cu（Ⅱ）、Co（Ⅱ）、Ni（Ⅱ）、Zn（Ⅱ）、Cd（Ⅱ）、Mn（Ⅱ）的行为。试验表明,Cu（Ⅱ）、Co（Ⅱ）、Ni（Ⅱ）在pH6～9范围内,与Zincon形成的螯合物可被Tween－80相完全萃取,而Zn（Ⅱ）、Cd（Ⅱ）、Mn（Ⅱ）基本不被萃取,进而实现了Cu（Ⅱ）、Co（Ⅱ）、Ni（Ⅱ）与Zn（Ⅱ）、Cd（Ⅱ）、Mn（Ⅱ）混合离子的定量萃取分离。     

中国化学会历届会长(理事长)、副会长(副理事长)、总干事(秘书长)

中国化学会成立时设理事9人,候补理事2人,理事会推举会长、书记、会计各一人,组成常务理事会。理事会受全体会员委托,决定本会的计划及处理各种会务。     

薄层色谱法测定痕量的镍(Ⅱ)、铜(Ⅱ)、镉(Ⅱ)、钴(Ⅱ)、锌(Ⅱ)的研究

在pH值为9.5～9.9的氨-氯化铵的缓冲溶液中,镍(Ⅱ)、铜(Ⅱ)、镉(Ⅱ)、钴(Ⅱ)、锌(Ⅱ)形成氨合络合物,而银(Ⅰ)、铋(Ⅲ)、铁(Ⅲ)、铁(Ⅱ)、汞(Ⅱ)、汞(Ⅰ)、锰(Ⅱ)、铅(Ⅱ)、锡(Ⅳ)、锡(Ⅱ)、钒(Ⅴ)、铝(Ⅲ)、钛(Ⅳ)等生成各种形式的沉淀。用甲醇-乙醇-氯化铵-氨-水体系(pH9.0～9.1),在硅胶H薄层板上,可以实现镍(Ⅱ)、铜(Ⅱ)、镉(Ⅱ)、钴(Ⅱ)、锌(Ⅱ)的分离。双硫腙显色后,用CS-930双波长薄层扫描仪测定含量。线性范围:锌0.01～0.20微克,铜0.01～0.25微克,镍、镉、钴0.01～0.30微克。     

柱后反应高效离子交换色谱法测定Cu(Ⅱ)、Zn(Ⅱ)、Ni(Ⅱ)、Co(Ⅱ)、Fe(Ⅱ)

目前,在无机离子交换色谱中,多使用电化学检测系统,今年我国也研制成了库仑检测器。我们应用了高效离子交换柱,实现了某些离子的分离;并选用了适当的螯合剂与流出组分进行了柱后螯合显色反应;用一般高效液相色谱仪常备的分光光度检测器,实现了某些无机离子的检测。这种方法既增强了检测某些离子的选择性,也提高了检测灵敏度。实践表明,用Partisil-10 SCX键合相离子交换柱进行分离,用水溶性二乙醇胺二硫代甲酸螯合剂为柱后反应试剂,检测波长为405毫微米,测得Cu(Ⅱ)、Zn(Ⅱ)、Ni(Ⅱ)、Co(Ⅱ)、Fe(Ⅱ)的检出限量为毫微克级。实验液相色谱仪Perkin-Elmer Series 3型,配有LC-65T紫外-可见分光光度检     

四元淋洗液的离子色谱法同时分离和测定铁(Ⅲ)、铁(Ⅱ)、铜(Ⅱ)、镍(Ⅱ)、锌(Ⅱ)、钴(Ⅱ)和铅(Ⅱ)

本文叙述了一种四元淋洗液同时分离和测定七种金属离子的色谱条件。探讨了各离子的保留行为与淋洗液pH值和络合剂浓度间的变化规律。方法用于镀铬槽液中金属杂质分析,相对标准偏差小于2.0％,相对误差不超过3.5％。     

茶叶、银杏叶中铅(Ⅱ)、镉(Ⅱ)、铜(Ⅱ)的测定

1　引　　言四 (4 磺酸苯基 )卟啉 (ＴＰＰＳ4)在最佳条件下可与Ｐｂ 、Ｃｄ 、Ｃｕ 形成稳定的络合物。但由于卟啉可与多种金属离子反应 ,因此 ,要将此络合物体系用于成分复杂的天然植物分析 ,则必须解决干扰问题。本文利用简便、易操作、不需使用大量有毒有机试剂及具有选择性吸附的巯基棉富集分离方法 ,实现了样品中干扰离子的分离以及痕量Ｐｂ 、Ｃｄ 、Ｃｕ 的富集和相互分离。此体系应用于茶叶、银杏叶中Ｐｂ 、Ｃｄ 、Ｃｕ 的测定 ,获得良好结果。2　实验部分2 .1　仪器和试剂　ＵＶ 2 4 0型紫外可见分光光度计 (日本岛津公司 …     

PVA-Fe(Ⅲ)、Zn(Ⅱ)、Cd(Ⅱ)、Hg(Ⅱ)配合物的合成、表征及抗菌性能

以聚乙烯醇(PVA)为高分子配体,与金属离子在溶液中进行配位反应,合成了PVA-Fe(Ⅲ)、PVA-Zn(Ⅱ)、PVA-Cd(Ⅱ)、PVA-Hg(Ⅱ)配合物.通过IR、Raman和XPS测试技术对配合物进行表征.IR结果显示,各配合物νc-o从纯PVA的1094cm-1向低波数方向移动8～11cm-1,νc-c由纯PVA的1430cm-1向低波数方向移动3～8cm-1;Raman显示,PVA-re(Ⅲ)、PVA-Zn(Ⅱ)、PVA-Cd(Ⅱ)、PVA-Hg(Ⅱ)配合物均在200～400cm-1处出现金属-氧键新峰;PVA-Fe(Ⅲ)的XPS显示O1s(533.0ev)、C1s(285.0eV)、Fe2p(712.0eV)的结合能与PVA[O1s(532.5eV)、C1s(284.6eV)]及FeCl3[Fe2p(711.2eV)]比较,发生了显著变化.以上结果表明,PVA分子侧链上的羟基氧提供孤对电子对与金属离子的空轨道形成配位键.配合物的抗菌实验结果显示,PVA-Hg(Ⅱ)对大肠杆菌、枯草芽孢杆菌和金黄色葡萄球菌具有很强的灭菌效果,PVA-Zn(Ⅱ)的灭菌效果较弱.     

Solvent-free synthesis of quinoline derivatives via the Friedländer reaction using 1,3-disulfonic acid imidazolium hydrogen sulfate as an efficient and recyclable ionic liquid catalyst

A convenient, highly versatile and eco-friendly protocol for the synthesis of quinoline derivatives via the Friedländer reaction is presented. The method is based on the use of 1,3-disulfonic acid imidazolium hydrogen sulfate (DSIMHS) as an efficient and reusable ionic liquid catalyst. A variety of ketones afforded the substituted quinolines in excellent yields during relatively short reaction times under solvent-free conditions; the catalyst could be easily recovered and reused for several times without any appreciable loss of activity.     

One-pot synthesis of various xanthene derivatives using ionic liquid 1, 3-disulfonic acid imidazolium hydrogen sulfate as an efficient and reusable catalyst under solvent-free conditions

In this study, 1,3-disulfonic acid imidazolium hydrogen sulfate （DSIMHS） is used as an efficient and reusable ionic liquid for the green, mild, and efficient synthesis of xanthenes under solvent-free conditions. Simple and easy work-up, low cost, green process, short reaction times and excellent yields of the products are the advantages of this procedure. Further, the catalyst can be recycled and reused at least for four times without a noticeably decrease in its catalytic activity.     

聚(4-乙烯基吡啶丁烷磺酸)硫酸氢盐:一个高效的多相聚(离子液体)固体酸催化剂用于无溶剂条件下一锅法合成1-酰氨基-2-萘酚和取代喹啉(英文)

Poly(4-vinylpyridinium butane sulfonic acid) hydrogen sulfate has been used as an efficient dual acidic catalyst for the one-pot preparation of 1-amidoalkyl-2-naphthols and substituted quinolines under solvent-free conditions.The catalyst was characterized by Fourier transform infrared spectroscopy, scanning electron microscopy, and thermo-gravimetric analysis. The results revealed several advantages to our new catalyst system,including its reusability,facile work-up procedure, eco-friendly reaction conditions,short reaction time,and high product yields.     

3-甲基-1-磺酸咪唑硫酸氢盐催化剂用于四组分一锅法合成不对称聚羟基喹啉衍生物(英文)

3-Methyl-1-sulfonic acid imidazolium hydrogen sulfate has been used as an efficient, halogen-free,and reusable Brnsted acidic ionic liquid catalyst for the synthesis of ethyl-4-aryl/heteryl- hexahydro-trimehtyl-5-oxoquinoline-3-carboxylates via the one-pot condensation of dimedone with aryl/heteryl aldehydes, ethyl acetoacetate, and ammonium acetate under solvent-free conditions. This method has the advantage of being clean and simple, as well as providing the desired product in high yield over a short reaction time. Furthermore, the catalyst could be recycled and reused four times without any discernible reduction in activity.     

Aluminum hydrogen sulfate [Al(HSO4)3] as an efficient catalyst for the preparation of thioacetals

Aluminum hydrogen sulfate, as a heterogeneous solid acid catalyst, has been used for the mild conversion of carbonyl compounds to their thioacetals using 1,2- and 1,3-dithiol under ambient conditions with short reaction times in high to excellent yield in acetonitrile as solvent.     

Polymer-supported gadolinium triflate as a convenient and efficient Lewis acid catalyst for acetylation of alcohols and phenols

A polymer-supported gadolinium triflate (CMPS-IM-Gd) catalyst was prepared from chloromethyl polystyrene (CMPS) resin using a simple and convenient procedure. This polymeric catalyst was used as an efficient Lewis acid catalyst for the acetylation of various alcohols and phenols with acetic anhydride, affording high yields under mild conditions. The reaction was completed in a short period of time with small amounts of the catalyst. The catalyst was reused over 10 times without any significant loss of its catalytic activity.     

无溶剂条件下N-磺酸琥珀酰亚胺催化乙酰化反应(英文)

A small amount of succinimide-N-sulfonic acid efficiently catalyzed the acetylation of a variety alcohols, phenols, thiols, amines and aldehydes with acetic anhydride at room temperature under solvent free conditions. This catalyst has the advantages of excellent yields and short reaction times and the reaction can be carried out on a large scale, which makes it potentially useful for industrial applications.     

硫酸氢钠催化合成阿魏酸戊酯的研究

以正戊醇和阿魏酸为原料,一水硫酸氢钠为催化剂,直接酯化合成了阿魏酸戊酯.考察了催化剂用量、反应时间、醇酸物质的量比、带水剂用量等因素对反应的影响.确定了较佳反应条件为:阿魏酸0.2mol,n(阿魏酸)∶n(戊醇)=1∶2,一水硫酸氢钠0.5g,环己烷(带水剂)15mL,加热回流反应2h,在此反应条件下阿魏酸戊酯的产率为96.9％.     

Polystyrene-supported GaCl3: A new,highly efficient and recyclable heterogeneous Lewis acid catalyst for acetylation and benzoylation of alcohols and phenols

A new, simple and highly chemoselective method for both acetylation and benzoylation of alcohols and phenols with acetic anhydride in the presence of polystyrene-supported gallium trichloride (PS/GaCl₃) as a highly active and reusable heterogeneous Lewis acid catalyst is presented. In this catalytic system, primary, secondary and tertiary alcohols as well as phenols were converted to the corresponding acetates and benzoates with high yields. The heterogenized catalyst is of high reusability and stability in the acetylation reactions and was recovered several times with negligible loss in its activity or a negligible catalyst leaching, and also there is no need for regeneration. Remarkably, a selective mono-acetylation of symmetrical diols can be achieved chemoselectively by employing the same catalyst.     

以聚(4-乙烯基吡啶)硫酸氢盐为催化剂三组分一锅法合成苯并[f]茚并喹啉(英文)

7‐Aryl‐8H‐benzo[f]indeno[2,1‐b]quinoline‐8‐one derivatives were synthesized by means of a one‐pot condensation of 2‐naphthylamine, aromatic aldehydes, and indane‐1,3‐dione in ethanol under refluxing conditions in the presence of poly(4‐vinylpyridinium) hydrogen sulfate, a solid acid catalyst. This method has the advantages of high yield, clean reaction, simple methodology, and short reaction time. The catalyst could be recycled and reused four times without significant loss of activity. The structure of the novel compounds was confirmed by IR, 1H NMR, and 13C NMR spec-troscopy and elemental analysis.