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1.
动力学分光光度法测定微量草酸的研究 总被引:5,自引:0,他引:5
本文详细讨论了草酸对锡-苯基荧光酮-溴化十六烷基三甲基铵三元络合物显色反应的催化动力学条件,建立了动力学光度法测定微量草酸的新方法,本法Sandell灵敏度为7.4ng/cm^2,草酸浓度在0-1.0μg/mL范围有良好线性关系,方法可直接用于菠菜中草酸含量的测定。 相似文献
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赵勤 《理化检验(化学分册)》1996,32(5):284-285,287
利用表面活性剂溴化十六烷基三甲基铵(CTMAB)的增敏作用,用火焰原子吸收光谱法测定了在氯化锶或氟化铵存在下精制铵明矾中痕量元素的含量,测定的灵敏度高,结果令人满意,回收率91% ̄109%,相对标准偏差(RSD)低于8.9%。 相似文献
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《理化检验(化学分册)》2010,(9)
在pH 3.1盐酸溶液和表面活性剂溴化十六烷基三甲基铵(CTMAB)存在下,铜(Ⅱ)对过氧化氢氧化甲基橙的褪色反应具有催化作用,在此基础上提出了测定痕量铜(Ⅱ)的催化分光光度法。由于添加了溴化十六烷基三甲基铵表面活性剂,灵敏度提高了2~3倍。铜(Ⅱ)的质量浓度在1.0×10-3~4.0×10-2mg.L-1范围内与ΔA呈线性关系。方法的检出限(3S/N)为4.6×10-4mg.L-1。该法用于河水中痕量铜(Ⅱ)的测定,并作回收试验,测得回收率为98.4%~103.0%,测得值的相对标准偏差(n=6)小于3%。 相似文献
4.
测定亚硝酸根的表面活性剂增敏催化动力学光度法 总被引:12,自引:1,他引:12
基于在稀硫酸介质中溴化十六烷基三甲基铵对NO2-催化溴酸钾氧化曙红褪色反应的作用,建立了测定NO-2的表面活性剂增敏催化动力学光度法。加入十六烷基三甲基溴化铵(CTMAB)后体系最大吸收波长由480nm红移至540nm,ΔA增大约20倍。ΔA与NO-2含量在001~02mg/L范围内存在线性关系,检出限为0004mg/L。方法已用于水样中NO-2测定,结果满意 相似文献
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1-(5-萘酚-7-磺酸)-3-[4-(苯基偶氮)苯基]-三氮烯的合成及与阳离子表面活性剂的显色反应 总被引:31,自引:0,他引:31
报道了1-(5-萘酚-7-磺酸)-3-[4-(苯基偶氮)苯基]-三氮烯(NASAPAPT)的合成,研究了该试剂与阳离子表面活性剂溴化十二烷基二甲基苄铵(DDMBAB),溴化十六烷基三甲铵(CTMAB)、溴化十六烷基吡啶(CPB)、溴化十四烷基吡啶(TPB)显色反应的条件。测定了显色反应的灵敏度,符合比尔定律的范围。建立了光度法测定微量阳离子表面活性剂的新方法。 相似文献
6.
偏最小二乘分光光度法同时测定痕量铁、锰、铜、锌、钴和镍 总被引:19,自引:0,他引:19
痕量Fe^3 ,Mn^2 ,Cu^2 ,Zn^2 ,Co^2 ,Ni^2 与2-(5-溴-2-吡啶偶氮)-5-二乙氨基苯酚(5-Br-PADAP)和溴化十六烷基三甲基铵(CTMAB)在PH8.3时发生高灵敏显色反应,所形成的三元胶束络合的吸收光谱严重重叠,采用偏最小二乘法(PLS)辅助分光光度法测定了合成试样及饲料中上述6种痕量组分,结果表明,PLS法是化学计量学中一种可适用于基体较复杂的实际试样中痕量组分分光度同时测定的多元计算方法。 相似文献
7.
抑制-催化褪色光度法测定痕量铬(Ⅲ) 总被引:6,自引:0,他引:6
提出一种测定痕量Cr(Ⅲ)新的抑制-催化动力学光度法。该法基于溴化十六烷基三甲铵于结晶紫在碱性介质中褪色反应的催化作用和Cr(Ⅲ)对此催化褪色反应的抑制效应。该法用于水样中Cr(Ⅲ)的测定结果满意。对有关该褪色反应的催化和抑制机理亦进行了讨论。 相似文献
8.
阳离子表面活性剂存在下锗与2,3,7-三羟基-9-取代萤光酮显色反应的研究 总被引:8,自引:0,他引:8
本文研究了八种2,3,7-三羟基-9-取代荧光酮在阳离子表面活性剂存在下与锗的胶束增敏显色反应.发现水杨基萤光酮及邻硝基苯基萤光酮在强酸性介质中可以和溴化十六烷基三甲基铵形成高灵敏的胶束三元配合物.较详细地研究了用邻硝基苯基萤光酮与溴化十六烷基三甲基铵分光光度法测定微量锗的实验条件.并探讨了有关配合物的组成以及胶束增敏反应的机理.此法可不经分离,直接快速测定铅锌矿中的微量锗,结果比较满意. 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
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.
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.
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.
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
19.
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
20.
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