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1.
报道了色谱301固载硫杂杯芳烃树脂分离预富集-火焰原子吸收光谱法测定痕量银的新方法。探讨了固载硫杂杯芳烃树脂对银的吸附原理与最佳条件。将含Ag^+试液在pH=10、温度为23±2℃的条件下恒温震荡10min,静置10min,Ag^+可被树脂定量富集被吸附的Ag^+可用5mL酸性硫脲(0.15mol/L HCl+0.15mol/L硫脲)完全洗脱,洗脱液中的银用火焰原子吸收光谱法测定。该法对银的检出限为0.17μg/L(3σ,n=11);线性范围为0.006—3mg/L。对0.18mg/L的Ag^+标液进行7次测定,RSD=1.53%。回收率在99.9%-105.0%之间。用于“二次资源”锌矿渣和环境水样中痕量银的测定,结果满意。 相似文献
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流动注射在线三正辛胺萃淋树脂分离富集火焰原子吸收法测定银 总被引:3,自引:0,他引:3
使用填充三正辛胺(TOA)萃淋树脂的微型柱,采用流动注射在线分离富集与火焰子吸收法联用技术,对微量银的测定进行了研究。在1.0mol/L HCl介质中样品流速为8.1mL/min,采样60s,以0.25mol/L HCl-0.5mol/L硫脲洗脱。在30样/h的分析速度下,富集倍率为26倍,富集效率为26/min,消耗指数为0.31mL。线性范围为0-1000μg/L,检出限为1.2μg/L。银含量为50μg/L时,连续11次测定的相对标准偏差为1.4%。对铅锌冶炼矿渣样液进行加标回收率试验,回收率为91.1%-100.6%,并应用于测定光谱纯氧化镁中的微量银。 相似文献
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以正十六胺-L113B-煤油为膜相,内相为0.040mol/L的NaOH溶液;外相为0.040mol/L的KCl和0.060mol/L的HCl溶液对痕量铊进行分离富集。实验结果表明,Tl(Ⅲ)的迁移率达99.5%以上。在合适的条件下,可与其它离子分离。此法可用于黄铁矿样品中微量铊的分离富集,以火焰原子吸收光谱法测定,回收率在99%以上。本文还对Tl(Ⅲ)的液膜富集机理进行了讨论。 相似文献
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PVC-PP树脂分离富集/火焰原子吸收光谱法测定海水中痕量铜镍钴 总被引:5,自引:0,他引:5
采用自制的聚氯乙烯多乙烯多胺(PVC-PP)树脂,在pH值为5.0的条件下,分离富集海水中的痕量铜、镍、钴,以1.2mol/L盐酸溶液洗脱.火焰原子吸收光潜法测定,富集倍数最大可达100倍(回收率大于90%)。研究了吸附与洗脱的最佳条件,方法检出限分别为铜0.81μg/L、镍0.98μg/L、钴0.57μg/L(富集倍数100,S/N=3),相对标准偏差小于5%(n=7),样品加标回收率在90%-105%之间。 相似文献
6.
固载硫杂杯芳烃树脂分离富集-火焰原子吸收法测定痕量银 总被引:5,自引:0,他引:5
报道了色谱301固载硫杂杯芳烃树脂分离预富集-火焰原子吸收光谱法测定痕量银的新方法。探讨了固载硫杂杯芳烃树脂对银的吸附原理与最佳条件。将含Ag 试液在pH=10、温度为23±2℃的条件下恒温震荡10min,静置10min,Ag 可被树脂定量富集被吸附的Ag 可用5mL酸性硫脲(0.15mol/LHCl 0.15mol/L硫脲)完全洗脱,洗脱液中的银用火焰原子吸收光谱法测定。该法对银的检出限为0.17μg/L(3σ,n=11);线性范围为0.006~3mg/L。对0.18mg/L的Ag 标液进行7次测定,RSD=1.53%,回收率在99.9%~105.0%之间。用于“二次资源”锌矿渣和环境水样中痕量银的测定,结果满意。 相似文献
7.
三聚氰胺-甲醛-三乙烯四胺树脂的合成及其对痕量银的吸附性能研究与应用 总被引:1,自引:0,他引:1
以甲醛为交联剂,以三聚氰胺、三乙烯四胺为原料合成了一种新型的三聚氰胺-甲醛-三乙烯四胺(MF-TETA)分离树脂,研究了MF-TETA分离树脂对痕量银的分离富集性能,探讨了MF-TETA分离树脂对银的吸附原理与最佳条件。在pH6.0、温度为35℃的条件下,试液中的银可被MF-TETA树脂定量吸附,其静态饱和吸附容量为32 mg/g,吸附在树脂上的银可用10 mL0.05 mol/L HNO3完全洗脱,洗脱液中的银用火焰原子吸收光谱法(FAAS)测定。该法对银的检出限为16 ng/mL(3σ,n=11),线性范围为0.05~5mg/mL,RSD=2.2%,回收率在95.8%~102.0%之间,方法可用于中草药中痕量银的测定。 相似文献
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地质样品中金银的连续快速测定——二苯硫脲-三正辛胺棉富集分离液珠萃取比色法 总被引:1,自引:0,他引:1
薛光 《理化检验(化学分册)》1999,(2)
采用二苯硫脲(DPTU)—三正辛胺(TNOA)棉富集分离金、银已有报道。本文采用该吸附剂制备了DPTU—TNOA棉吸附柱,并研究了动态法富集分离金、银的条件。研究表明.吸附柱富集金、银的最佳酸度(体积分数)为5%~20%王水。当含金溶液以1~6ml·min~(-1)流速通过0.1g吸附剂制备的吸附柱时,金、银的吸附率均在98%以上。采用硫代米蚩酮(TMK)液珠萃取比色法连续测定了地质样品中的金、银。方法的检出限为0.5×10~(-9),银为5×10~(-9)。经样品验证,其分析结果满足化探找金工作的需要。 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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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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Synthesis of substituted pyrrolo[1,2-a]pyrazines and pyrazino[1,2-a]indoles from the Morita-Baylis-Hillman derivatives of acrylates via saponification followed by Curtius reaction is described. 相似文献
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用正丁胺作为碳源,采用射频辉光放电制备碳膜,选用激光染料R6G和聚乙二醇混合液作为蒸气源,采用单源热蒸发,在蒸发室与染料同时沉积得到混合膜,用拉曼光谱和红外光谱分析了碳膜的结构和键合方式,分析表明:碳膜中存在胺基团和氢原子.混合膜的荧光谱测量结果表明,认为正丁胺对染料荧光谱的影响是因为胺基和氢原子的存在. 相似文献
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Jona Mirnik Eva Pušavec Kirar Sebastijan Ričko Uroš Grošelj Amalija Golobič Franc Požgan Bogdan Štefane Jurij Svete 《Tetrahedron》2017,73(24):3329-3337
A series of 20 CuAIAC reactions between eight 4-acylamino substituted pyrazolidine-3-one-1-azomethine imines and four terminal ynones were performed using Cu0 as catalyst. The corresponding fluorescent cycloadducts were obtained in very high yields upon simple workup. Thus, Cu-metal turned out to be a better catalyst than CuI in terms of yield and ease of isolation. Availability of azomethine imines, mild reaction conditions, and simple workup enable a “click” access to libraries of densely substituted 2,3-dihydro-1H,5H-pyrazolo[1,2-a]pyrazol-1-ones. Reactivity of differently substituted dipoles was evaluated experimentally and by quantum chemical methods (DFT). 相似文献
20.
George E. Magoulas Thomas Garnelis Constantinos M. Athanassopoulos Dionissios Papaioannou George Mattheolabakis Konstantinos Avgoustakis Dimitra Hadjipavlou-Litina 《Tetrahedron》2012,68(35):7041-7049
(E)-4-(Fullerenopyrrolidin-1-yl)-3-methylbut-2-enoic acid and its corresponding succinimidyl ester, readily obtained through Prato-type modification of C60, were used for the selective N-acylation of polyamines. The thus obtained conjugates were evaluated for their antioxidative and anti-inflammatory activity and their cytotoxicity was determined. Members of this family of compounds showed interesting anti-lipid peroxidation, anti-lipoxygenase and anti-inflammatory activity and comparable cytocompatibility to spermidine. 相似文献