截流分光光度法

观测快速溶液反应的尝试，始于1923年，Roughton采用连续流动法，用热电偶测定血红朊和一氧化碳的结合速度。1940年Chance Gibson提出了截流法，用小量试样来观测过氧化氢酶或过氧化物酶与过氧化氢的反应，然后在溶液高速反应上广泛应用。另一方面酸碱的中和反应质子移动反应和氧化还原电子移动反应，则于1953年由Eigon提出了缓和法（化学驰豫）即改变温度、压力、     

分光光度分析

本文是本刊“分光光度分析”的定期评述的继续 ,主要是对 1 998年 6月～ 2 0 0 0年 6月年间我国在分光光度分析领域中的研究现状及进展进行了评述。文献资料主要来自国内主要杂志和全国性学术会议 ,对我国学者在国际杂志上发表的论文也给予部分收录。内容包括专著、综述、学术会议、有机试剂及多元络合物体系、动力学光度法、其它光度分析法 (固相光度法、导数光谱 ,双波长分光光度法及化学计量学光度法 )和流动注射在光度分析中的应用 (包括流动注射荧光法及化学发光法 )。引用文献 32 1篇     

721型分光光度计分光系统常见故障的排除

721型分光光度计分光系统的常见故障有无出射单色光或光斑不完整、单色光波长指示值与实测值不一致、波长调节器转动时出射光波长无变化、波长调节器转动困难且波长读数盘不动等，分析了造成这类故障的原因，并阐述了排除这类故障的方法。     

导数分光光度法

前言在进行分光光度分析时,通常面临下述二个方面的问題。即: 1.外来物质与主成份吸收带相互重叠,干扰对待测物质的鉴别和测定。 2.在测定波长范围内,辐射光受到溶剂、胶体、悬浮体等的散射或吸收,减弱了直达检测器的光强,降低了分析性能。对此,传统的方法大多采用诸如过滤、沉淀、蒸馏、萃取和色谱等化学和物理化学分离手段来消除影响。近些年来,利用改进测试仪器性能克服上述局限性的努力已收到显著的效果。虽然,使用某一仪器进行测量所获得的基本信息量不随输出方式而有实质性变化。但是,输出信息的     

高灵敏度无机分光光度法

前言对于分析方法,特别是工业分析方法,一般都希望不使用价格昂贵的特殊装置;操作简便;不论何人、何时、何地使用均能得到可靠的数据。而分光光度法在相当程度上能满足这样的要求。虽然现在各种仪器分析方法得到了迅速的发展,但分光光度法仍然广泛应用于各个领域,日本工业标准等法定的分析方法亦采用分光光度法,其原因恐怕就在于此。如果能将分光光度法韵应用范围从以往的痕量成分分析扩大到超痕量成分分析,那将是非常理想的。从这个观点出发,     

差示分光光度法

測量溶液吸收度的方法目前,比色分析(严格地說应称为吸收分析)在广泛地被应用着,由于近代仪器和技术上的发展,这种方法除了用直接法測量一般吸收度,以測定微量成分外,还能对吸收度过高(高浓度)或吸收度过低(低浓度)的溶液进行測量,以測定物貭中某一含量較高或过低的成分。在适当条件下,可以获得相当滿意的結果,其中对高含量(可达90％以上的成分)的測定而言,有时可达与重量或容量分析同等的精确度。根据使用溶液調节透光度标尺讀数为“0”和“100”     

721型分光光度计

721型分光光度计是综合我厂原来生产的72型分光光度计、551型双光比色计、583型浦氏光度计等三种仪器的技术指标,并保持其各项优点,改革不合理的结构而制造的一种新产品,仪器的电源部分,单色器,比色部分以及测定读数部分全部装合成一件,便于操作。 721型分光光度计(见图1)可供工厂、矿山、医院以及科研单位的试验室在可见光谱区范围内进行一般的比色分析,仪器具有足够的光量调节范围,可采用有     

分光光度法测定头孢氨苄

头孢氨苄与茚三酮在酸性水溶液中能发生显色反应。表观摩尔吸光系数为是７．９５×１０＾３Ｌ．ｍｏｌ＾－１．ｃｍ＾－１。作者详细研究了该反应的条件，应用拟定的方法测定药物制剂含量与药典方法一致，回收率在９９％以上。     

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.     

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.     

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.