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1.
碘化物-结晶紫-聚乙烯醇体系分光光度法测定自来水中痕量二氧化氯 总被引:6,自引:0,他引:6
在稀磷酸介质中,二氧化氯(ClO2)氧化I离子形成 I3配阴离子,I3进一步与结晶紫(CV)阳离子形成离子缔合物[CV][I3」。在聚乙烯醇存在下,该离子缔合物最大吸收波长λmax位于552 nm处,摩尔吸光系数ε=25 × 105L·mol-1·cm-1,对 ClO2的检出限为 0.6 μg/L,线性范围是 0.6~280μg/L。加入适量 KF溶液可消除自来水中Fe(Ⅲ)的干扰。方法对μg/L级ClO2 的测定有较好的选择性,可成功地用于自来水样品分析。 相似文献
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在六次甲基四铵-盐酸介质中, 痕量铬(Ⅵ)显著催化H2O2氧化‘花青褪色的指示反应, 催化反应的表观活化能为6.84 kJ·m ol- 1, 建立了测定痕量铬(Ⅵ)的动力学分析法, 线性测定范围为0~150 μg·L- 1,检出限为0.8μg·L- 1。常见离子中,除Al3+ ,Cu2+ ,Fe3+ ,Fe2+ 外,其余离子不影响测定。其中Al3+ 的干扰可用F- 掩蔽消除, Cu2+ ,Fe3+ ,Fe2+ 的干扰可用EDTA 掩蔽消除。本法已用于测定湖水,矿井水和电镀废水中的铬(Ⅵ)。 相似文献
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一阶导数吸光光度法同时测定纯硅中铁和铝的研究 总被引:4,自引:0,他引:4
提出了用一阶导数光光度法同时测定铁和铝的方法,在pH6.5乙二胺缓冲溶液中,乳化剂OP存在下,Fe^3+Al^3+与络天青S形成Fe^3+,Al^3+-CAS-OP三元络合物,络合物一阶导数光谱等吸收点分别在606.2,638.0nm记录混合体系在两波长处一阶导数数值可以分别测定铝,铁含量,互不影响,铁,铝含量分别在1.0~16μg/25ml,0.3~10μg/25ml范围内呈良好线性,用于测定纯 相似文献
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分光光度法同时测定中草药中的钼和铜 总被引:2,自引:2,他引:2
本文建立了在混合显色剂(PF+PAN)的胶束体系中,利用分光光度法同时测定中草药中的钼和铜。实验表明:在混合体系中,钼量在0~10μg/25mL,铜量在0~50μg/25mL的范围内符合比尔定律,ε′Mo=9.2×104L·mol-1·cm-1;ε′Cn=1.5×104L·mol-1·cm-1。该法用于中草药样品的分析,结果满意,回收率可达92~111%。 相似文献
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在硫酸介质中,在过量碘化钾及阿拉伯胶存在下,IO-3氧化I-生成I-3,I-3再与结晶紫形成离子缔合物,缔合物的最大吸收波长为552nm,表观摩尔吸光系数ε552=5.38×105L·mol-1·cm-1,IO-3量在0~12μg/25mL范围内服从比耳定律.用于生物样品中碘的测定,结果满意 相似文献
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本文报道一种新的测定δ-氨基乙酰丙烯(δ-ALA)的分光光度法,方法基于δ-ALA被缩合成吡咯衍生物后,在酸性条件与Fe^3+生成橙红色配合物,其λmax为480nm,ε为6.6×10^3L.mol^-1.cm^-1,线性范围10~400μg/25mL,回收率94~104%。 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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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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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-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
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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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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. 相似文献
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