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1.
火焰原子吸收光谱法间接测定非金属材料中氯 总被引:9,自引:0,他引:9
报道了火焰原子吸收光谱法(FAAS)间接测定非金属材料中氯的方法,采用AgCl沉淀,测定剩余Ag~+间接求出氯含量。方法的特征浓度为0.014mg/L(1%吸收),检出限为0.032mg/L(3),测定下限为0.11mg/L,相对标准偏差(RSD)为1.5%~10%,样品加标准回收率在91.4%-105%之间。 相似文献
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偏最小二乘催化极谱法同时测定铂,钯,铑 总被引:6,自引:0,他引:6
应用M273A电化学系统中的线性扫描技术,确定了0.75mol/LH2SO4-1.5%NH4Cl-2.8mmol/L(CH2)6N4-0.0025%N2H4.H2SO4为偏最小二乘极谱法同时测定Pt、Pd、Rh的最佳极谱体系。Pt、Pd、Rh的线性范围为3.2mg/L、0-15.0mg/L和0-1.0mg/L。模拟样品及实际样品的回收率在90.3-107.7%之间。 相似文献
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芦荟大黄素的电化学研究 总被引:8,自引:1,他引:8
用单扫示波极谱法研究了芦荟大黄素的电化学行为。在5%Na2CO3+5%NaOH(9+1)底液中,芦荟大黄素于-0.84V(P1)和-0.97V(P2)处产生两个示波极谱峰,利用P1可测定芦荟大黄素,线性范围为 0.11-24mg/L和3.0-28.6mg/L,检测限为0.06mg/L。将该法应用于中药大黄中的芦荟大黄素的测定,结果满意。另外,讨论了芦荟大黄素清除由邻苯三酚自氧化产生的超氧自由基(O2)的作用。 相似文献
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离子色谱法测定固体颗粒中可溶性阴离子 总被引:4,自引:0,他引:4
选用HPIC-As-4A离子色谱分离柱及AFS-2纤维抑制双柱系统,使用Na2CO3-NaHCO3双组份为淋洗液,采用电导检测器,利用峰高、峰面积法定量分析。F-(0.02~0.7)、Cl-(0.3~1.0)、NO-3(0.05~0.2)、SO2-4(0.6~2.0mg/L)范围内,其校正曲线有很好的线性关系,相关系数均在0.9984~0.9998。应用此方法分析了大气总悬浮颗粒物和粉煤灰陶粒试样中可溶性阴离子,获得了可靠的分析结果。NO-3、SO2-4回收率分别为93.90%、101.9%。 相似文献
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抑制动力学分析法测定痕量铈 总被引:11,自引:0,他引:11
1引言研究了铈(Ⅲ)阻抑H2O2氧化水杨基荧光酮(SAF)褪色的反应。反应对铈(Ⅲ)为一级反应,表观活化能为28.75kJ/mol。据此建立了测定痕量铈的动力学分析法。测定条件为:SAF:4.0x10-5mol/L,H2O2:0.010%,NaOH:2.0x10-2mol/L,50℃。线性范围0.04~0.44mg/L,检测限为0.02mg/L。当溶液中的铈含量为0.16mg/L时,3~8倍量的轻稀土,5~11倍量的重稀土及同倍量铀和钍不干扰测定。2实验部分2.1试剂和仪器铈(Ⅲ)标准溶液:20… 相似文献
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1-(4-硝基苯基)-3-[4-(苯基偶氮)苯基]-三氮烯-溴化十六烷基三甲铵-阴离子表面活性剂显色反应的研究及应用 总被引:2,自引:0,他引:2
在三乙醇胺存在下,1-(4-硝基苯基)-3-[4-(苯基偶氮)苯基]-三氮烯(Cadion)与溴化十六烷基三甲铵(CTMAB)和阴离子表面活性剂(AS)形成红色配合物,其最大吸收位于550nm。改变阴离子表面活性剂十二烷基苯磺酸钠、十二烷基磺酸钠、十二烷基硫酸钠时,有色配合物的表观摩尔吸光系数ε550分别为3.02×104、2.13×104、2.94×104(Lmol-1cm-1),阴离子表面活性剂服从比尔定律的范围分别为0~4.18mg/L,0~2.18mg/L,0~3.46mg/L。方法用于测定环境水样中阴离子表面活性剂,结果满意 相似文献
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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
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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
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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
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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
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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
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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
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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
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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
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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
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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