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原子荧光光谱法测定食品中的镉 总被引:7,自引:0,他引:7
研究了在水溶液中,Cd与KBH4反应生成挥发性物种,以原子荧光光谱法测定食品中的痕量Cd的分析方法,方法的检出限为0.12μg/L,线性范围0~50μg/L,回收率为86%~112%。 相似文献
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以酒石酸-乙二胺为淋洗液的单柱离子色谱法同时测定磷酸中痕量钠(Ⅰ)和铁(Ⅲ)。淋洗液最佳浓度为4.0mmol.L ̄(-1)、酒石酸/1.0m mol·L ̄(-1)乙二胺。最低检测限为Na ̄+0.05μg/mL、 Fe3+ 0.45μg/mL。电导检测灵敏度为2.0μg/cm。线性范围Na ̄+、Fe3+0.2~1.5×103μg/mL、2.5~1.0×103μg/mL。相对平均偏差Na ̄+为2.03%、Fe3+为0.83%。平均回收率Na ̄+为98.26%、Fe3+为97.62%。本法简便、快速、准确、选择性好。 相似文献
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固氮蓝藻分离富集石墨炉原子吸收光谱法测定痕量Cr(Ⅵ)/Cr(Ⅲ) 总被引:5,自引:0,他引:5
本文选取固氮蓝藻分离富集Cr(Ⅵ)/Cr(Ⅲ),用墨炉原子吸收光谱法测定。结果表明该方法对10mL试样,测定Cr(Ⅵ)的检测限为0.1μg.L^-1'变异系数为3.2%,在0-45μg.L^-1范围内线性关系好;测定Cr(Ⅲ)的检测限为0.3μg.L^-1、变异系数3.7%,在0-40μg.L^-1范围内线性关系好。方法选择性高、富集率高。测定矿泉水、海水及自来水中的铬,获得满意结果。 相似文献
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氢化物发生电感耦合等离子体原子发射光谱法同时测定水和生物样品中… 总被引:13,自引:0,他引:13
研究了一种小型同心氢化物发生配置一个气液分离器后与多道ICP-AES联用,同时测定水和生物样品中砷、铋、锑、硒的方法。检出限为砷0.4μg/L,铋0.5μg/L,锑1.4μg/L,硒0.5μg/L,相对标准偏差为砷2.7%,铋1.5%,锑2.7%,硒1.9%。用本法测定美国和国家标准物质中的氢化元素,结果满意。 相似文献
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1引言以碱性染料光度法同时测定磷、砷、硅已有报道,但需加入掩蔽剂或经还原-萃取等分离。本文用三波长K系数法原理,由计算机选出最佳波长组合,不经分离、掩蔽,于一份试液中同时测定痕量磷、砷、硅,其线性范围分别为40.0~240.0μg/L、32.0~120.0μg/L、32.0~320.0μd/L。用于合成样品测定,结果令人满意。2实验部分2.1仪器与试剂722型光栅分光光度计。硅标准溶液:用高纯SiO2(99.99%)以常法熔融配成pH约1.5的溶液,含硅0.100g/L;磷标准溶液:用KH2PO… 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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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
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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
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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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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
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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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Microwave-assisted copper-catalyzed ring expansions of three-membered heterocycles with α-diazo-β-dicarbonyl compounds were investigated. Thiiranes generated 3-acyl-5,6-dihydro-1,4-oxathiines in the presence of copper sulfate and trans-3-acyl-5,6-dihydro-1,4-oxathiines as stereospecific products for 1,2-disubstituted cis-thiiranes through an intramolecular SN2 process. Oxiranes gave rise to 2-acyl-5,6-dihydro-1,4-dioxines under the catalysis of copper hexafluoroacetylacetonate and cis-3-acyl-5,6-dihydro-1,4-dioxines as stereospecific products for 1,2-disubstituted cis-oxiranes via an intimate ion-pair mechanism. The current method provides a direct and simple strategy in efficient preparation of 3-acyl-5,6-dihydro-1,4-oxathiines and 2-acyl-5,6-dihydro-1,4-dioxines, important agents in medicinal and agricultural chemistry, from readily available thiiranes and oxiranes, respectively. 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