固相萃取光度法测定饮用水中的酚

1　引　　言酚类物质是水样中重要污染物之一 ,水中酚含量达 0 .1～ 0 .2ｍｇ Ｌ时会导致生长的鱼虾有异味 ,浓度大于 5ｍｇ Ｌ时会导致水生物中毒死亡。世界卫生组织规定饮用水中挥发酚最高浓度为 0 .0 2ｍｇ Ｌ理想值为 0 .0 1ｍｇ Ｌ。目前ＧＢ74 90 87采用蒸馏分离 ,4 氨基安替比林显色后用三氯甲烷萃取光度法测定水中的挥发酚。该方法操作麻烦 ,易污染环境 ,而且对于浓度低于 0 .0 2ｍｇ Ｌ,难于富集到光度法测定的线性范围 ,由于酚类物质易氧化 ,在蒸馏过程中易造成损失而影响测定结果。我们研究了用 4 氨基安替比林直接显色 ,固相…     

水体中邻苯二酚和对苯二酚检测方法的研究进展

邻苯二酚和对苯二酚是水体中重要的污染物,对生物体具有严重的危害作用,故实现邻苯二酚与对苯二酚的快速简便、灵敏高效的检测具有十分重要的意义.本文作者综述了近几十年来国内外检测邻苯二酚和对苯二酚的主要方法,如色谱法、分光光度法、化学发光法和电化学分析方法,阐述了各种检测方法的特点;并探讨了两种物质的检测方法的发展趋势.     

还原偶氮分光光度法测定水中硝基苯方法的改进

<正>还原偶氮分光光度法测定水中硝基苯[1-3],是污水、废水污染监测中一个重要的分析方法,具有仪器简单、灵敏度高和普及性强等特点,是硝基苯类有机化学污染物监测不可缺少的方法之一。但在运用该方法进行实际样品分析时,发现该方法在样品氧化还原前处理过程中操作比较繁琐,且易造成样品损失。针对这个问题,本工作对氧化还原前处理装置进行了改进[4],取消了前处理装置,使样品的氧化还原前处理和定容一步到位;简化了操作,提高了试验     

环境水质中酚类优先监测物的气相色谱法测定

以气相色谱法（ＧＣ）测定了环境水质中的重点酚类污染物。选择乙酸酐作衍生化试剂、甲苯为萃取剂,比较了不同的衍生ｐＨ条件,给出了氢火焰离子化检测器（ＦＩＤ）分离测定酚类污染物的精密度和检出限。方法简便实用,经５家实验室验证表明：适用于监测地表水和污水中的酚类物质。６种酚类优先监测物的检测限为０．６～７μｇ／Ｌ。     

气相色谱-邻苯二甲酸二甲酯内标法同时测定硝基苯酚的三种异构体

酚类已被列为优先控制的环境污染物,属高毒物质,其中硝基苯酚的3种异构体的分析测定备受关注。目前,已有采用分光光度法[1]、离子色谱法[2]、高效液相色谱法[3]测定的报道,但未查阅到采用气相色谱法对硝基苯酚的3种异构体同时分离和测定的系统研究。本文采用乙酸酐衍生化法对3种酚进行衍生,使之成为酯类进行分离[4],并采用邻苯二甲酸二甲酯作为内标物进行定量分析。1　实验部分1.1　主要仪器与试剂　　美国Agilent6890气相色谱仪,氢火焰离子化检测器(FID),HPRev.A.08.01化学工作站;HP 5毛细管柱。邻、间、对硝基苯酚及乙酸酐、甲苯…     

地质环境样品中挥发酚分析现状与进展

挥发酚被列为环境优先控制的有机污染物,已成为评价环境污染的重要指标之一。该文简述了挥发酚的化学性质及地质环境来源,概括了国内外挥发酚测定的相关标准方法,从样品预处理技术和检测技术两方面综述了近年来地质环境样品中挥发酚分析的研究现状。重点对溶剂萃取、蒸馏、固相萃取、固相微萃取和吹扫捕集等样品预处理技术,以及4-氨基安替比林分光光度法、紫外和荧光分光光度法、溴化容量法、气相色谱法、液相色谱法和酚生物传感器法等技术在地质环境样品中挥发酚分析上的应用进行了较为全面的总结,并对其未来的发展趋势进行了展望,为进一步研究挥发酚的分析技术及其环境应用提供参考。     

食品及环境样品中双酚类物质的前处理及检测方法研究进展

双酚类物质作为一种环境内分泌干扰物,广泛存在于食品包装材料及环境介质中,对生态环境造成污染,也对人体健康产生一定危害。双酚残留是目前重要的食品安全问题,检测食品和环境样品中的双酚类物质的含量对人体健康具有重要的意义。由于残留目标物浓度通常较低,且实际样品存在基质干扰,因此需经一定的样品前处理,并结合仪器分析方法,提高检测效率,增强分析灵敏度与可靠性。常用的前处理分析方法主要有液液萃取、微波辅助萃取、固相萃取、固相微萃取、基质分散固相萃取、QuEChERS等,常用仪器分析方法包括液相色谱法、气相色谱法、毛细管电泳法、酶联免疫吸附测定法、生物传感器法等。该文综述了食品及环境样品中双酚类物质的样品前处理及仪器分析方法,为双酚类化合物的残留监测提供了参考依据。     

流动注射安培法测定水中总氰化物

氰化物是一种广泛存在于自然界的剧毒物质,工业用途十分广泛,如湿法冶炼金、银等,主要污染源为电镀、炼焦、选矿、有机、化工、化肥等工业污水[1-2]。目前国内测定总氰化物的方法主要有硝酸银滴定法、分光光度法、电极法、色谱法等[3]。传统的化学法检测氰化物需蒸馏预处理,而且显色时还需水浴恒温,操作繁琐、费时、费力。流动注射安培法具有分析速度快、操作简单、样品和试剂消耗少等优点,已应用于环境、农业等领域中氰化物的检测。     

紫外分光光度法测定2,4-二氯苯酚

2,4-二氯苯酚被世界野生动物基金会列为潜在的内分泌修正化学物质,即环境荷尔蒙物质.这类物质在环境中虽然含量低,但却显示出超常的内分泌效应,因而对其的监测分析显得尤为重要.目前,分析2,4-二氯苯酚的方法有比色法[1]和色谱法[2].色谱法虽然快速、准确,但对仪器要求高,操作复杂,而比色法灵敏度低.用紫外分光光度法测定河水中的2,4-二氯苯酚.     

苯胺极谱测定新方法及其机理研究

苯胺是环境污染物对人体有一定毒害并可致癌，印染和制药厂排放废水含苯胺尤多，通常用条乙二胺偶氮光度法测定．该法用于测定有色或含酚量高的工业废水时，程序复杂，周期长［1］．用导数示波极谱法测定操作繁琐，酚类干扰严重［2］．我们在实验中发现，苯胺在酸性介质中...     

二氧化碳和丙烯直接合成甲基丙烯酸的NiPMo/TiO2催化剂的研究

用溶胶-凝胶法以磷钼酸(MPA)的镍盐溶液水解钛酸四丁酯制备了NiPMo/TiO2催化剂.使用ICP、 XRD、 TG-DTA、 IR、 TPD-MS和微反应技术研究了催化剂的化学组成、热稳定性、化学吸附性质和催化反应性能.杂多钼酸盐与TiO2通过O2-在TiO2表面发生了键合.在623 K下,杂多阴离子仍保持原有的Keggin结构.CO2在Lewis酸位Ni(Ⅱ)和Lewis碱位Ni-O-Mo的桥氧协同作用下生成CO2卧式吸附态Ni(Ⅱ)←O-(CO)←(O--Ni).丙烯有多种吸附态在催化剂上吸附.在563 K、 1 MPa和空速1500 h-1的反应条件下,丙烯的摩尔转化率为3.2%,产物MAA选择性为95%.     

Synthesis of 1-benzyloxypyrazin-2(1H)-one derivatives

Different approaches for the synthesis of 1-benzyloxypyrazin-2(1H)-one derivatives from simple amino acids have been investigated. A library of 33 precursors for the preparation of N-hydroxy pyrazinones was obtained in moderate to good yields.     

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.     

A general and convenient synthesis of 4-(tosylmethyl)semicarbazones and their use in amidoalkylation of hydrogen,heteroatom, and carbon nucleophiles

A general synthesis of previously unknown semicarbazone-based α-amidoalkylating reagents, 4-(tosylmethyl)semicarbazones, has been developed. The synthesis involved three-component condensation of semicarbazones of aliphatic or aromatic aldehydes with the same or other aldehydes and p-toluenesulfinic acid. The scope and limitations of this reaction were investigated. The compounds obtained were demonstrated to be an efficient α-(4-semicarbazono)alkylating agents. They were reacted with H- (sodium borohydride), O- (sodium methylate), S- (sodium phenylthiolate), N- (pyrrolidine, sodium succinimide), P- (trialkyl phosphites), and C-nucleophiles (sodium diethyl malonate) to give the corresponding products of the tosyl group substitution, 4-substituted semicarbazones, including analogues of nitrofurazone. Among the prepared compounds tested in vitro for antibacterial and antifungal activity, three nitrofuryl-containing semicarbazones exhibited high biological activities with minimum inhibitory concentration (MIC) values of 8–32 μg/mL.     

Synthesis of novel chiral bidentate hydroxyalkyl-N-heterocyclic carbene ligands and their application in palladium-catalyzed Mizoroki–Heck couplings and asymmetric addition of diethylzinc to benzaldehyde

A small library of new chiral bidentate hydroxyalkyl-imidazolium salts 1 is conveniently synthesized on multi-gram scale from inexpensive and commercially available chiral pool amino acids. The corresponding carbenes, generated by deprotonation of imidazolium salts 1, in combination with palladium(II) chloride were tested in the Mizoroki–Heck coupling reaction. The most significant results in terms of yields and reactivities were achieved with low catalyst loading. The catalytic activities of these imidazolium salts were also investigated in the asymmetric addition of diethylzinc to benzaldehyde. The use of MgO nanoparticles as an additive in conjunction with these ligands played a crucial role in increasing the efficiency of these reactions.     

Toward new camptothecins. Part 6: Synthesis of crucial ketones and their use in Friedländer reaction

In the context of the preparation of camptothecin and luotonin A analogs, the synthesis of some key keto-precursors and their use in Friedländer condensation are described. This paper also focuses on the stability of these keto intermediates and emphasizes the major differences between indolizinones and pyrroloquinazolinones series. Noteworthy is also the report of some original structures isolated as by-products of some experiments.     

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.