抗坏血酸为阻断剂肾上腺素法测定微量元素对SOD活性的影响

Vitamin阻断法测定了不同浓度Se、Mn、F- 对SOD活性的影响。结果显示 :①Se浓度由0 0 0 μg·L- 1增加到 40 0 μg·L- 1时 ,SOD活性由 5 1 0 0u·mg- 1上升到 5 40 0u·mg- 1;Se浓度继续增加到 60 0 μg·L- 1,SOD活性下降至 5 1 40u·mg- 1;②Mn浓度由 0 0 0 μg·L- 1增加到 40 0 μg·L- 1,SOD活性由 5 1 0 0u·mg- 1上升到 5 90 0u·mg- 1;Mn浓度继续增加到 5 0 0 μg·L- 1,SOD活性下降到 5 2 0 0u·mg- 1;③F- 浓度由 0 0 0 μg·L- 1增加到 1 0 0 μg·L- 1,SOD活性由 5 1 0 0u·mg- 1上升至 5 2 80u·mg- 1,继续增加F- 浓度到 2 0 0 μg·L- 1,SOD活性下降为 5 1 70u·mg- 1,再增加F- 浓度到 40 0 μg·L- 1,60 0μg·L- 1,80 0 μg·L- 1,SOD活性基本维持在 5 2 0 0～ 5 1 80u·mg- 1之间     

四元Mg0.9Ti0.1Ni0.9X0.1(X=Mn,Zn,Co,Fe)系列合金的制备及性能研究

用机械合金化法合成了Mg0·9Ti0·1Ni0·9X0·1(X=Mn,Zn,Co,Fe)系列合金.X射线衍射(XRD)结构分析表明,用X部分替代Ni后,促进了Mg0·9Ti0·1Ni合金的非晶化过程.用Co和Fe部分替代Ni提高了合金的放电容量,但却降低了合金的循环稳定性.用Zn和Mn部分替代Ni提高了合金电极的循环寿命,尤其是Mg0·9Ti0·1Ni0·9Zn0·1合金电极经10个充放电循环后,其放电容量仍可达到313·8mA·h/g.对添加Co后的合金进行p-c-T测试发现,Mg0·9Ti0·1Ni0·9Co0·1合金的吸放氢容量明显比Mg0·9Ti0·1Ni合金高,这与电化学所测到的结果一致.     

双波长吸光光度法同时测定多巴和酪氨酸的研究

研究了双波长吸光光度法同时测定多巴和酪氨酸。在 pH 1 2 .0 0的硼砂 氢氧化钠缓冲介质中 ,多巴和酪氨酸的含量分别在 0～ 2 0 .0 μg·ml-1和 0～ 1 9.0 μg·ml-1范围内呈良好线性关系 ,方法检出限和摩尔吸光系数 :多巴为 0 .2 3 μg·ml-1和 1 .2 0× 1 0 4L·mol-1·cm-1,酪氨酸为 0 .2 7μg·ml-1和 1 .48× 1 0 4L·mol-1·cm-1,方法的灵敏度和和选择性均较好 ,应用于尿液中多巴和酪氨酸的测定。     

钴-锌试剂络合吸附伏安法测定中草药中钴

研究了测定痕量钴的一种灵敏的吸附伏安法 ,利用钴和锌试剂络合物在悬汞电极上的吸附性 ,有效地提高了分析的灵敏度。在 0 .0 0 5mol·L-1NH3 和 0 .0 6mol·L-1NH4Cl及 2 .5× 1 0 -6mol·L-1锌试剂底液条件下 ,该体系 1 .5 ,2 .5阶微分吸附伏安法测定钴的线性范围为 1× 1 0 -10 ～ 1× 1 0 -7mol·L-1,用 2 .5阶微分吸附伏安法 ,富集 3min的检出限为 5× 1 0 -11mol·L-1。用此法直接测定了中草药中痕量钴     

催化动力学光度法测定食品中微量铜的研究

提出了催化动力学吸光光度测定铜的新方法 ,基于在 0 .0 5～ 0 .0 9mol· L-1硫酸介质中和 2 .0× 1 0 -3 mol·L-1氯化十六烷基吡啶存在下 ,Cu( )催化抗坏血酸还原邻甲氧基苯基重氮氨基偶氮苯。用固定时间法在 50 2 nm处监测催化反应。方法的线性范围为 0～ 2 8ng·ml-1,检出限( 3σ)为 0 .66ng· ml-1,摩尔吸光系数为 9.65× 1 0 5L· mol-1· cm-1。除 Fe( )外常见离子都不干扰测定。用 NH4 F掩蔽 Fe( ) ,方法直接应用于多种食品分析 ,结果与二乙基二硫代氨基甲酸钠萃取光度法相同 ,相对标准偏差为 2 .0 %～ 4.4% ( n=6)。非催化反应和催化反应在 3.0～ 8.0 min内为假零级反应 ,活化能分别为 1 56.1和 1 0 3.8k J· mol     

AgDDC光度法测定砷的探讨

砷是环保、卫生防疫等部门的一个重要分析项目。目前 ,Ag DDC光度法测定砷用得比较普遍。1　试验部分1 .1　仪器与试剂72 2分光光度计 ;1 0 0 ml测砷装置氯化亚锡溶液 :40 0 g·L-1碘化钾溶液 :1 50 g· L-1吸收液及以上试剂按文献 [1 ]配制砷标准溶液 (国家一级标准物质 GBW0 861 1 ) :1 mg· ml-1;砷中间液 :1 0 .0μg· ml-1;砷工作液 :1 .0 0μg· ml-1。无砷锌粒甲 :1 0～ 2 0目无砷锌粒乙 :颗粒较大 ,约绿豆大小。1 .2　试验方法在砷化氢发生瓶中加入砷工作液 (或水样适量 ) ,加水至 50 ml。分别加入浓硫酸 4ml,碘化钾溶液 4ml和…     

硅钡钙联合测定

硅钡钙是炼钢中很好的新型脱氧剂 ,并且有很好的脱硫、磷能力 ,对冶炼含硫、磷较低的钢种起着非常重要的作用 ,在特钢系统有着广阔的应用前景。本文提出了硅钡钙联合测定分析方法 ,该法快速、准确、简便、易掌握。1　试验部分1 .1　试剂混合熔剂 :无水碳酸钠 硼砂 过氧化钠 =2 0 1 0 3,硼砂在 350°C马弗炉中烘去结晶水分。NH4 CNS:50 g· L-1Ag NO3溶液 :1 0 g·L-1(NH4 ) 2 SO4 溶液 :1 0 0 g·L-1Ba Cl2 溶液 :1 0 0 g·L-1KOH溶液 :40 0 g·L-1EDTA标准溶液 :0 .0 2 mol· L-1,称取 EDTA基准试剂 7.4452 g溶于水中 ,用…     

高效液相钴离子催化化学发光抑制法测定茶叶中的茶氨酸

 研究了用高效液相分离、抑制化学发光测定茶叶中茶氨酸的分析方法。该法采用YWG C18(10μm,250mm×5 0mmi d )柱,以0 01mol·L-1醋酸钠 醋酸缓冲液(pH5 5)为流动相,流速为0 8mL·min-1。对茶氨酸抑制Co2+催化鲁米诺(luminol)与过氧化氢(H2O2)化学发光反应的条件进行了优化:Co2+的质量浓度为2μg·L-1,鲁米诺浓度为0 25mmol·L-1,H2O2浓度为0 5mmol·L-1。在茶氨酸的质量浓度为0 2g·L-1～5 0g·L-1时,茶氨酸抑制化学发光产生负峰的相对峰面积Y(将实际峰面积缩小至万分之一)与其质量浓度X(kg·L-1)的线性回归方程为Y=33862X+1 0605(r=0 9983)。     

硫代硫酸根的溶出伏安吸附性质及应用

在 0 .0 1mol·L-1LiNO3介质中 (pH 2 .70 )S2 O32 -有一灵敏的阴极溶出峰( - 0 .42V) ,其峰电流与S2 O32 -浓度在 1× 1 0 -7mol·L-1～ 4× 1 0 -6mol·L-1范围内有线性关系。当富集 2 0 0s时 ,检测限可达 5× 1 0 -8mol·L-1。溶出峰具有吸附性质 ,在悬汞电极上的吸附符合Frumkin等温式。测得在悬汞电极上的饱和吸附量为 1 .0 3× 1 0 -9mol·cm-2 。该方法用于PbS2 O3溶度积的测定 ,结果与文献值基本一致。     

关于配位滴定测定水的总硬度终点返红问题的讨论

ＥＤＴＡ滴定法测定水的总硬度时 ,常以 0 .1ｍｏｌ·Ｌ-1氨 氯化铵缓冲液调节溶液ｐＨ为 1 0 ,以络黑Ｔ为指示剂 ,用 0 .0 1ｍｏｌ·Ｌ-1ＥＤＴＡ滴定。此方法使用过程中经常出现终点返红问题。本文对此进行了试验。1　试验部分1 .1　主要仪器与试剂ＣＯ2 发生器 (自制 )氨 氯化铵缓冲溶液 :0 .1ｍｏｌ·Ｌ-1所用试剂均为分析纯以上1 .2　试验方法取自来水样 1 0 0 .0ｍｌ,以 0 .1ｍｏｌ·Ｌ-1氨 氯化铵缓冲液调节其 ｐＨ为 1 0 ,加络黑Ｔ指示剂 (与ＮａＣｌ配比为 1∶1 0 0 )少许 ,以 0 .0 1 0 0 0ｍｏｌ·Ｌ-1ＥＤＴＡ标准溶液滴定至终点…     

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.     

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.     

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.     

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.     

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.     

Chemistry of heterocyclic compounds at the A. E. Favorsky Irkutsk Institute of Chemistry, Siberian Branch of the Russian Academy of Sciences, over 50 years (Review)

The review contains a concise historical account and information on the most significant researches undertaken by the staff at the A. E. Favorsky Irkutsk Institute of Chemistry, Siberian Branch of the Russian Academy of Sciences on the Chemistry of Heterocyclic Compounds. Dedicated to Academician of the Russian Academy of Sciences B. A. Trofimov on his 70th jubilee. Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 10, pp. 1443–1502, October, 2008.     

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.     

Sulfur-directed metal-free and regiospecific methyl C(sp3)–H imidation of thioanisoles

Regiospecific and direct imidation of the methyl C(sp³)–H bond of thioanisoles is realized under mild and metal-free conditions with N-fluorobis(benzenesulfonyl)imide as an oxidant and nitrogen source. Proposed mechanism suggests that thionium ion intermediates and a Pummerer-type reaction are involved. The imidation has advantages such as high step-economy, excellent functionality tolerance, and regiospecificity, giving structurally diverse imidation products.     

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.