纺织品中残留氯酚的毛细管气相色谱测定法

采用稀硫酸浸湿样品,正己烷提取,乙酸酐衍生后以毛细管气相色谱分离测定的方法对纺织品中五氯酚、三氯酚残留量进行了同时测定,探讨了提取、净化及色谱分析条件。方法回收率范围三氯酚84.8％～98.1％,五氯酚88.0％～100.2％。相对标准偏差三氯酚1.54％～2.33％,五氯酚3.48％。方法的检出限（质量分数）分别为2,4,6-三氯酚1.0×10     

高效毛细管电泳—电化学检测对废水中优先监测酚类的测定研究

高效毛细管电泳－电化学检测法对６种中国环境优先监测的酚类进行了测定研究，考察了各实验参数对分离、检测的影响。在选定的最佳实验条件下，２５ ｍｉｎ内基线分离了上述 ６种酚类。测得浓度检测限（ｍｇ／Ｌ）：苯酚 ０． ０１；间－甲酚 ０．０１；２，４－二氯酚 ０．０６； ２，４，６－三氯酚０．０８；五氯酚０．１２；对硝基酚０．０７。本方法对实际废水样品中酚的测定结果满意。     

用超临界流体萃取和固相萃取分析水中酚类污染物

使用自制的超临界流体萃取仪，比较了从Ｃｈｒｏｍｏｓｏｒｂ，Ｐｏｒａｐａｒｋ和ＧＤＸ系列的８种吸附剂上萃取苯酚，邻硝基酚，邻氯酚，对氯酚，对二甲酚，２，４－二氯酚和２，４，６－三氯酚的回收率。并用萃取回收率比较高的ＧＤＸ－３０１富集１Ｌ酸性水样中１０＾－７ｇ／ｍＬ级的以上各酚，然后用超临界ＣＯ２脱附，回收率从３２．５％到９２．９％，同时还对超临界ＣＯ２脱附ＧＤＸ－３０１上各酚的操作条件进行了优化，并     

离子交换膜对采用生物膜电极法降解五氯酚的影响

以五氯酚（PCP）为目标污染物,在隔膜式电解槽中研究了不同离子交换膜对采用生物膜电极法处理五氯酚的影响. 结果表明,阴离子交换膜有利于五氯酚在生物膜电极上的转化和中间产物的去除;与生物法和电化学法降解五氯酚相比,采用以钛基二氧化铅为阳极（Ti/PbO₂）、生物膜电极为阴极、阴离子交换膜为隔膜的电解槽处理时,五氯酚的降解效果明显优于生物法和电化学方法,经24 h处理后五氯酚的去除率和化学需氧量（COD）去除率均可达到96%（质量分数）.     

几种挥发性有机酚的离子淌度谱测定

应用离子淌度谱仪在负高压方式下测得苯酚、２－氯代酚、２，４－二氯代酚及五氯代酚的折合淌度值分别为２．１２、２．０１、１．９３、１．７４ ｃｍ２Ｖ－１ｓ－１，检测限分别为 １．０、０．１、０．５、０．５μｇ／Ｌ，２－氯代酚、２，４－二氯代酚的二聚体的折合淌度值分别为 １．６０、１．４７ｃｍ２Ｖ１ｓ１，并对苯酚、２－氯代酚和２，４－二氯代酚的混合物进行了分析测定，并讨论了淌度值与分子量、分子形状之间的关系。     

串联质谱法快速分析皮革中五氯酚残留

建立了皮革样品中五氯酚的串联质谱分析方法,以ｍ／ｚ２６６为母离子,碰撞电压为０．８Ｖ,以子离子ｎ／ｚ２３０为定量离子,外标法定量。线性范围为０．１￣１０．０ｍｇ／Ｌ,检出限为０．００５ｍｇ／ｋｇ,回收率为８５．４％￣１０２．５％,相对标准偏差为２．５５％￣３．５５％。方法具有快速、准确的特点。     

固相微萃取/GC直接测定废水中的三种氯酚

研究了运用固相微萃取／GC直接测定水中的三种氯酚的方法，得到了分析三种氯酚的SPMF最佳萃取条件。选取聚丙烯酸酯（PA）萃取头，水溶液调pH=2,并用NaCl饱和，室温下在持续磁力搅拌下直接萃取40min，纤维萃取头在260℃脱附5min。所建立的方法适于快速、方便地测定水中三相氯酚，无须浓缩和预处理。     

超高效液相色谱-高分辨质谱确证分析泥鳅体内五氯酚代谢物

建立了超高效液相色谱-高分辨质谱(UPLC-HRMS)鉴定泥鳅体内五氯酚代谢物五氯酚磺酸酯的方法。将在低浓度五氯酚下暴露的泥鳅样品粉碎,采用含8%(体积分数)三乙胺的70%(体积分数)乙腈水溶液提取,经混合阴离子交换小柱萃取净化,在ACQUITY BEH C18色谱柱(100 mm×2.1 mm,1.7μm)上分离,采用电喷雾负离子(ESI-)一级质谱全扫描加数据依赖的二级质谱扫描(full mass-ddMS2)模式测定,获得代谢物的准分子离子、同位素离子和二级质谱碎片离子的精确质量数。结果表明,五氯酚在泥鳅体内的代谢以磺化为主,没有发现羟基化和葡萄糖醛酸化。代谢物主要为五氯酚磺酸酯,其含量随着暴露时间(t)的延长逐渐增加,当暴露时间为36 h时达到峰值,随后逐渐减小,当t≥120 h时,五氯酚磺酸酯含量基本维持不变。该方法可用于生物体内五氯酚的代谢研究。     

树脂吸附法处理五氯酚钠生产废水

本文用大孔吸附树脂ＣＨＡ—１１１处理五氯酚钠（ＰＣＰ—Ｎａ）生产废水，其中ＰＣＰ—Ｎａ含量为１００００～１５０００ｍｇ／Ｌ，ＣＯＤｃｒ高达１１０００ｍｇ／Ｌ。经中和沉淀－树脂吸附法处理，处理量为１２ＢＶ，吸附流出液中五氯酚（ＰＣＰ）含量≤１．１ｍｇ／Ｌ，ＰＣＰ去除率＞９９％，ＣＯＤｃｒ总去除率≥８０％，树脂脱附液经酸化处理，可回收ＰＣＰ。     

几种挥发性有机酚的离子淌度谱研究

篱子淌度谱仪在负高压方式下测得苯酚、２－氯代酚、２，４－二氯代酚及五氯代酚的折合淌度值分别为２．１２、２．０１、１．９３、１．７４ｃｍ＾２Ｖ＾－１ｓ＾－１，检测限分别为１．０、０．１、０．５、０．５μｇ／Ｌ，２－氯代酚、２，４－二氯代酚的二聚体折合沿度值分别为１．６０、１．４７ｃｍ＾２Ｖ＾－１Ｓ＾－１，并对苯酚、进行了分析测定，并讨论了淌度值与分子量，佞子形状之间的关系。     

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%.     

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.     

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.     

CoFe2O4自形成磁性液体场致结构化对磁化的影响

The Langevin paramagnetic theory can’t describe the relation between magnetization of ferrofluids and applied magnetic field. The structuralization of ferrofluids, which is considered the main influence factor of the magnetization, is regarded. The part of magnetization works is deposited when the structure is forming. This action influences the magnetization of ferrofluids directly or indirectly. On the base of the “compressing” model, the Langevin function that usually describes the magnetization of ferrofluid is modified, and a well-fitted curve is obtained. An equation of the relation between the equivalent volume fraction after being “compressed” and the intensity of magnetic field is discovered, which approximately describes the process of magnetization. The relation between the approximate initial susceptibility and the volume fraction can be obtained from modified formula.     

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.     

KMnO4-mediated oxidative CN bond cleavage of tertiary amines: Synthesis of amides and sulfonamides

KMnO₄-mediated oxidative CN bond cleavage of tertiary amines producing secondary amine was introduced, which was trapped by electrophiles (acyl chloride and sulfonyl chloride) to form amides and sulfonamides. The reaction could take place at mild condition, tolerating a wide range of function groups and affording products in moderate to excellent yields.     

Highly regioselective Buchwald–Hartwig amination at C-2 of 2,4-dichloropyridine enabling a novel approach to 2,4-bisanilinopyridine (BAPyd) libraries

The highly regioselective Buchwald–Hartwig amination at C-2 of the cheap and readily accessible reagent, 2,4-dichloropyridine with a range of anilines and heterocyclic amines is described. This new methodology is robust and provides a facile access to 4-chloro-N-phenylpyridin-2-amines on 0.25 mol scale. These intermediates undergo a further Buchwald–Hartwig amination at higher temperature to enable rapid exploration of the chemical space at C-4 and to provide a library of 2,4-bisaminopyridines.