共查询到20条相似文献,搜索用时 417 毫秒
1.
金在脱乙酰壳多糖学修饰电极上的电化学行为及分析应用 总被引:3,自引:1,他引:2
用脱乙酰壳多糖化学修饰电极为工作电极,阳极溶出伏安法测定痕量金。在pH1 ̄2的KCl-HCl底液中,超始电位0.20V,终止电位1.30V,富集时间5min,以-0.1/s扫速阳极溶出,峰电位在1.00V(vs.SCE),Au(Ⅲ)浓度在0.10mg/L ̄10mg/L范围内与峰高呈线性关系。在富集10min时,可检测0.25mig/LAu,大大提高了测定灵敏度,用于矿样测定,无需分离,结果满意。用 相似文献
2.
3.
Nafion修饰金电极阳极溶出伏安法测定痕量碲 总被引:4,自引:0,他引:4
本文用Nafion修饰金盘电极,在0.04mol/LLiCl和PH2的H2SO4底液中,阳极溶出伏安法测定痕量碲,研究了富集溶出过程的特性和优化条件,碲浓度在0.2-15ng/mL范围内与溶出峰电流呈良好的线性关系。本法灵敏度高,选择性好,用于测定小麦粉和玉米粉中痕量碲,测定标准偏差小于0.07μg/g,与ICP测定结果比较其相对误差小于16%。 相似文献
4.
蒙脱石修饰碳糊电极测定氨基酸的研究:Ⅱ.酪氨酸的测定 总被引:13,自引:1,他引:13
本文报道蒙脱石修饰碳糊电极测定酪氨酸,在0.001mol/L KCl-HCl(pH=2.0)溶液中开路富集,介质交换后微分脉冲阳极溶出伏安法测定,在0.5-2.5μg/ml范围内有线性,检测限为63ng/ml。可避免其他氨基酸,微量元素和常量金属元素的干扰,直接用于氨基酸药物样品的分析,获得了满意的结果,还对酪氨酸在电极上的反应机理进行了探讨。 相似文献
5.
6.
7.
8.
药物分子在玻碳电极电的电分析化学研究:Ⅳ.乙酰螺旋霉素的伏安测定 总被引:2,自引:0,他引:2
本文对乙酰螺旋霉素在GCE上的伏安行为进行了研究,发现在磷酸盐缓冲溶液(pH=7.78)中,於+0.85V(vs,Ag/AgCl)左右产生一良好的阳极氧化伏安峰,浓度在0.5~100μg/mL之间与峰电流呈线性关系,分析了制剂中乙酰螺旋霉素的含量,相对标准偏差为4.5%,平均回收率为101%,经循环伏安法验证,电极反应为不可逆反应。 相似文献
9.
应用循环伏安法、微分脉冲伏安法对多菌灵在破碳电极上的电化学行为及其测定进行了研究。在pH=9.0的2mol/L NH3-NH4Cl底液中,对其进行循环伏安扫描,发现于0.61V(vs.Ag/AgCl)产生一灵敏的氧化峰。微分脉冲伏安法殉菌灵的检测限为4×10^-8mol/L。多菌灵的浓度在5.0×10^-7 ̄1.0×10^-5mol/L间与微分脉冲伏安峰电流呈线性关系(r=0.9942)。对于1× 相似文献
10.
单扫描极谱法连续测定人发中的微量元素锌铁锰铜 总被引:3,自引:0,他引:3
本提出在0.15mol/L乙二胺-7.5×10^-3mol/L三乙醇胺-2.5×10^-2mol/L硫氰酸钾底液中单扫描极谱法测定锌、铁、锰,续加硫酸(0.3mol/L)测定铜的方法,峰电位分别为-1.42V,-1.63V,-1.71V,-0.48V(vs.SCE),线性范围:0.05~1.4μg/mLMn,0.04~1μg/mLCu,最低检出浓度.03,0.05,0.02,0.04μg/mLM 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.
Toward new camptothecins. Part 6: Synthesis of crucial ketones and their use in Friedländer reaction
Laurent Gavara Thomas Boisse Jean-Pierre Hénichart Adam Daïch Philippe Gautret 《Tetrahedron》2010,66(38):7544-5571
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
13.
Uroš Grošelj Mojca Žorž Amalija Golobič Branko Stanovnik Jurij Svete 《Tetrahedron》2013,69(52):11092-11108
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.
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. 相似文献
16.
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. 相似文献
17.
Rebecca J. Burton Mandy L. CrowtherNeal J. Fazakerley Shaun M. FilleryBarry M. Hayter Jason G. KettleCaroline A. McMillan Paula PerkinsPeter Robins Peter M. SmithEmma J. Williams Gail L. Wrigley 《Tetrahedron letters》2013
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. 相似文献
18.
N. A. Nedolya 《Chemistry of Heterocyclic Compounds》2008,44(10):1165-1219
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. 相似文献
19.
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
20.
Shashikant U. Dighe Surya K. Samanta Shivalinga Kolle Sanjay Batra 《Tetrahedron》2017,73(17):2455-2467
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