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1.
宋俊峰  高雅芳 《分析化学》1995,23(4):438-441
本报道一种测定哌仑西平的单扫描示波极谱法,在0.1mol/LNH4Cl-NH3.H2O(pH8.0±0.1)缓冲液中,哌仑西平有一极谱还原波,其峰电位为-1.51V(vs.SCE),其一阶导数峰高与哌仑西闰浓度在6.6×10^-7-4.6×10^-6mol/L(r=0.9981)和6.6×10^-6-1.6×10^-5mol/L(r=0.9991)范围内有线性关系,检测限为3.4×10-7mol  相似文献   

2.
环氧化植物油的制备   总被引:4,自引:0,他引:4  
天然油脂在无溶剂加压(约0.15MPa)条件下,经甲酸(85%)、双氧水(50%)环氧化,一步合成增塑剂兼稳定剂环氧化油脂,得微黄色油状透明液体;环氧大豆油和环氧葵子油的环氧值均在6.2%~6.6%,环氧玉米油的环氧值6.0%~6.4%;碘值小于3mg/g;精油转化率104%~108%。  相似文献   

3.
合成了3种以4,4’-联吡啶为配体的三核环状Cu(Ⅱ)配合物[Cu3(4,4'-bpy)3.(phen)3](ClO4)6.2H2O(1),[Cu3(4,4'-bpy),(bpy)3](ClO4)6.H2O(2)和[Cu394,4'-bpy)3.(NO2-phen)3](ClO4)6.6H2O(3)。经元素分析,电导,IR,电子光谱,ESR,磁化率等方法进行了表征,推定该配合物具有以4,4’-联吡  相似文献   

4.
研究了反应物配料比3-AMP/Cl(摩尔比)、反应温度与时间对大孔型3-氨甲基吡啶树脂(3—AMPR)性能的影响规律.在最佳合成工艺条件下制得3-AMPR的功能基含量为3.16mmol/g树脂.3-AMPR对AuCl6(2-),PtCl6(2-),IrCl6(2-),PdCl4(2-),RhCl6(3-)的吸附容量分别为800.8,387.8,386.3,133.0,105.5mg金属/g树脂;配位比分别为1.29,0.63,0.64,0.40,0.33。比较了3—AMPR、2-AMPR、4-氨基吡啶树脂(4-APK)、3—APR、2-APR五种树脂对AuCl4-、PtCl6(2-)的吸附性,其中3-AMPR为最佳。  相似文献   

5.
方禹之 《分析化学》1998,26(6):694-697
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。  相似文献   

6.
胡顺兴 《大学化学》1994,9(3):33-34
在铵盐存在下,莫尔法滴定时酸度的计算胡顺兴(福建南平师范专科学校福建353000)有存在时,莫尔法的滴定酸度,国内权威教科书上都有明确的示值,pH为6.5~7.2[1-4],但也有的教科书指出,实验证明值的pH为6.0~7.0[5]。经查文献[6],...  相似文献   

7.
提出了一个简便测定微量镉的灵敏的示波极谱法,在pH=4.0的HAc和少量非离子型表面活性剂存在下,Cd(Ⅱ)产生一灵敏的极谱波,峰电位为-0.67V,线性范围为2.0×10-8mol/L~4.9×10-6mol/L,检出限为5.6×10-9mol/L.该法用于废水样及发样的测定,结果良好  相似文献   

8.
汽车氢化物空调机用贮氢合金的研究   总被引:1,自引:0,他引:1  
针对汽车发动机尾气废热为驱动热源的应用要求,研究了一对新的稀土系贮氢合金对La0.6Ml0.4Ni4.7Cr0.8-La0.2Mm0.8Ni4.35Fe0.65。该合金对在150~250℃/35~45℃/15~20℃工作温度下做制冷循环时,最大工作氢容量为4.5H/molM,理论特性系数COPc为0.74,可基本满足氢化物空调机应用要求。  相似文献   

9.
在0.06mol/L柠檬醚钠-0.003mol/LHC1(pH6.5)介质中,2,3,4-三羟基-4′-磺基-偶氮苯和铋产生灵敏的单扫描极谱导数峰,铋含量在0~6.7×10 ̄(-6)mol/L范围内与波高成线性关系,检测限2.4×10 ̄(-8)mol/L。用提出的方法测定了锡中的铋,并对反应机理进行了研究。  相似文献   

10.
食品中酪氨酸含量的测定   总被引:7,自引:3,他引:7  
运用酪氨酸与4-氨基安替吡啉的显色反应测定食品中酪氨酸的含量,微波加热水解30s后,可在不分离其它氨基酸的条件下直接测定酪氨酸,向5mL的水解液中依次加入5ml5.0×10^-2mol/L4-氨基酸安替比林,2.5mLNH4OH-NH4Cl缓冲溶液(pH9.40),2.5mL0.1mol/L高碘到溶液,用二次水定容于50mL,显色25min后,以空和参比,在480nm波工下测定吸光度值,深度估6.  相似文献   

11.
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%.  相似文献   

12.
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.  相似文献   

13.
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.  相似文献   

14.
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.  相似文献   

15.
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.  相似文献   

16.
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.  相似文献   

17.
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%).  相似文献   

18.
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.  相似文献   

19.
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.  相似文献   

20.
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.  相似文献   

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