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1.
动力学—两次标准加入法同时测定钼和钨 总被引:4,自引:3,他引:4
本文提出了动力学-两次标准加入法双组份同时测定的新方法,讨论了测定的基本原理;用停流FIA光度法研究了钼和钨共同催化的H2O2-I^-动力学反应体系,并建立了钼和钨同时测定的条件,用本法测定了钢样和模拟样品中的钼、钨含量,结果满意,钼和钨的回收率分别为97%-102.6%和98.2%-103%;相对标准偏差分别为2.8%-3.2%和2.1%-3.5%。 相似文献
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酵素菌肥的金属元素营养分析 总被引:1,自引:0,他引:1
在磷酸根、硅酸根存在下以2%硝酸镧作机体改进剂,测定了酵素菌肥中多种金属元素的含量,各元素的平均回收率分别为:K98.69%,Ca100.37%,Mg97.81%,Na96.06%,Cu98.26%,Fe96.45%,Zn99.78%,Sr93.54%,Li94.22%。方法简便,快速可靠,肯定 酵素菌肥的金属元素营养价值。 相似文献
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高效液相色谱法分析矿泉水中酚类化合物 总被引:23,自引:1,他引:22
用带荧光检测器的高效液相色谱法同时测定了矿泉水中的苯酚、甲酚、双酚A、双酚F、4-叔丁酚、双酚A二环氧甘油醚和双酚F二环氧甘油醚等,水样经液-固萃取浓缩后再进行分析,检测限可达0.1~0.2μg/L。重复测定的标准偏差为1.12%~13.21%,水样测定的回收率为81%~105%。 相似文献
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北京近郊土壤中痕量半挥发性有机污染物的分析方法研究 总被引:24,自引:0,他引:24
利用超声提取、吸附色谱分离以及气相色谱和气-质谱联用的方法对土壤中痕量半挥发性有机污染物进行了提取、分离以及定性定量分析。优化了硅胶和弗罗里土吸附净化正构烷烃和多环芳烃以及有机氯农药和酞酸酯类化合物的分离条件。正构烷烃、多环芳烃、有机氯农药和酞酸醑的平均回收率分别为82%-105%、103%~110%、94%-117%和86%-l14%;检出限分别为3—22、3—42、0.004—0.088和10—220ng/g;相对标准偏差均小于15%。本方法用于分析北京近郊土壤中的上述有机污染物,经质量控制分析,结果可靠。 相似文献
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凌梅秀 《广东微量元素科学》2005,12(2):15-17
为了解信宜市城区幼儿园儿童体内微量元素含量情况,回顾性分析了2003年信宜市城区幼儿园3至7岁儿童头发微量元素普查资料。结果表明,本区儿童缺锌率20.42%,缺碘率14.26%,缺钙率8.86%,缺铁率3.00%,铅高率42.04%。提示该市城区幼儿园儿童体内微量元素失衡相当普遍,必须加强幼儿园管理,监测和指导儿童微量元素营养,开展健康教育,提高群卫生保健意识,普通城区也要开展儿童铅中毒防治工作。 相似文献
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测定人血清白蛋白的荧光光纤流动免疫分析系统 总被引:5,自引:2,他引:3
用新型荧光光纤免疫传感流动分析测试系统,对人血清白蛋白(HSA)进行测试;将偶联于微晶纤维素表面形成的HSA固相抗体与待测HSA(抗原)、荧光标记抗原(FTTC-HSA)竞争性结合。经稀碱液处理,固相载体与抗原抗体复合物分离,用新型荧光光纤免疫传感流动分析系统测定解析液的荧光值,以求得待测HSA的含量;该法检出限为0.1g/L,日内RSD0.91%-6.4%,日间RSD1.8%-8.0%,加标回收率91%-120%;用该法测定注射用HSA,与临床检验常用的溴甲酚绿化对照,具有良好的相关性(r=0.9808)。 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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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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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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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
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N. A. Nedolya 《Chemistry of Heterocyclic Compounds》2008,44(10):1165-1219
The review contains a concise historical account and information on the most significant researches undertaken by the staff
at the A. E. Favorsky Irkutsk Institute of Chemistry, Siberian Branch of the Russian Academy of Sciences on the Chemistry
of Heterocyclic Compounds.
Dedicated to Academician of the Russian Academy of Sciences B. A. Trofimov on his 70th jubilee.
Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 10, pp. 1443–1502, October, 2008. 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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《Tetrahedron》2014,70(21):3377-3384
The Rh(II)-catalyzed reaction of 2-carbonyl-substituted 2H-azirines with ethyl 2-cyano-2-diazoacetate or 2-diazo-3,3,3-trifluoropropionate provides an easy access to 2H-1,3-oxazines and 1H-pyrrol-3(2H)-ones. These compounds can be selectively prepared from the same starting material using temperature as the only varied parameter. The 2-azabuta-1,3-diene intermediate, a common precursor for both heterocyclic products, isomerizes into 2H-1,3-oxazine under kinetic control, while 1H-pyrrol-3(2H)-one is the sole product of the reaction at elevated temperatures. According to DFT-calculations a one-atom oxazine ring contraction involving ring-opening to a 2-azabuta-1,3-diene intermediate, followed by a 1,5- and 1,2-prototropic shift leads to the consecutive formation of imidoylketene and azomethine ylide, which then further undergo cyclization to the pyrrole derivative. 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