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开缝石英管原子捕集原子吸收光谱法测定银 总被引:3,自引:0,他引:3
试验了空气和乙炔流量、缝管高度、捕集时间、溶液介质等对银灵敏度的影响。结果表明,分别用不同的乙炔流量进行原子捕集与释放可获得最高灵敏度。捕集1min,测得银的特征浓度为8.1×10~(-4)μg·ml~(-1),比常规火焰原子吸收法的灵敏度提高62倍,变异系数2.8%,本法测定了牡蛎中的银。 相似文献
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原子捕集—火焰原子吸收法测定工业废水中痕量镉 总被引:3,自引:0,他引:3
1 引言 原子捕集是在火焰原子吸收测量中浓缩待测原子的一种预富集手段。以往的报道原子捕集管多用石英材料,选用不锈钢材料作捕集管测镉的方法尚未见报道。本文系统研究了使用不锈钢管作捕集管,各种因素对镉捕集与释放的影响,选择了最佳工作条件。捕集3min测镉的特征浓度为1.52×10~(-4)μg/ml/1%,灵敏度比常规法提高了116倍。相对标准偏差为1.5%。而且不锈钢管具有坚固耐用的优点。本法用于工业废水中痕量镉的测定,获得满意结果。 相似文献
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赵进沛 《广东微量元素科学》1995,2(3):33-36
采用自制原子捕集装置,选择了镉在不锈钢管上捕集的合适条件,使测镉的灵敏度比常规火焰原子吸收法提高了116倍。应用于工业废水中痕量镉的测定,获得满意结果。 相似文献
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浊点萃取-石英双缝管捕集火焰原子吸收光谱法分析铬价态 总被引:2,自引:0,他引:2
在不同pH值的缓冲溶液中,亚硝基苯胲铵盐(铜铁试剂)可与Cr(Ⅵ)及Cr(Ⅲ)络合生成中性疏水络合物,以Triton X-114为萃取剂,浊点萃取分离富集Cr(Ⅵ)及总铬,石英双缝管原子捕集-火焰原子吸收光谱法(STAT-FAAS)测定铬价态.实验对浊点萃取时溶液的pH值、铜铁试剂和Triton X-114的用量、离心分离时间、平衡温度和时间等影响因素进行了研究.结果表明,分别在pH=3.0和6.0的溶液中,40 ℃恒温加热15 min后,离心5 min,Triton X-114浊点萃取Cr(Ⅵ)及总铬的富集倍数达到50倍(100 mL起初样品溶液/2 mL最终测定液).和普通火焰原子吸收光谱法(FAAS)相比,利用石英双缝管原子捕集技术,STAT-FAAS法测定铬的灵敏度提高了近5倍.本方法测定Cr(Ⅵ)及总铬的线性范围分别为0.005~0.5 mg/L和0.01~1.2 mg/L;检出限分别为0.66 μg/L和0.81μg/L. 相似文献
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原子捕集原子吸收光谱法测定银的研究 总被引:3,自引:1,他引:3
West等人用硅管在空气-乙炔焰中捕集银2分钟,测得银的特征浓度为9×10~(-4)ppm,比常规火焰原子吸收法的灵敏度提高40倍。孙汉文用不锈钢管在空气-乙炔焰中捕集0.005ppm银10分钟,测得银的特征浓度为4×10~(-4)ppm。根据原子捕集和释放机理,本文改进了实验装置和方法,即采用贫焰捕集,脉冲富焰释放的方法,在石英捕集管上捕集0.001ppm银溶液8分钟,测得银的特征浓度为5.5×10~(-5)ppm,比常规方法的灵敏度提高1090倍。初步测定了电镀液中银含量。 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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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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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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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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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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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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