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1.
宋俊峰  高雅芳 《分析化学》1995,23(4):438-441
本报道一种测定哌仑西平的单扫描示波极谱法,在0.1mol/LNH4Cl-NH3.H2O(pH8.0±0.1)缓冲液中,哌仑西平有一极谱还原波,其峰电位为-1.51V(vs.SCE),其一阶导数峰高与哌仑西闰浓度在6.6×10^-7-4.6×10^-6mol/L(r=0.9981)和6.6×10^-6-1.6×10^-5mol/L(r=0.9991)范围内有线性关系,检测限为3.4×10-7mol  相似文献   

2.
环氧化植物油的制备   总被引:4,自引:0,他引:4  
天然油脂在无溶剂加压(约0.15MPa)条件下,经甲酸(85%)、双氧水(50%)环氧化,一步合成增塑剂兼稳定剂环氧化油脂,得微黄色油状透明液体;环氧大豆油和环氧葵子油的环氧值均在6.2%~6.6%,环氧玉米油的环氧值6.0%~6.4%;碘值小于3mg/g;精油转化率104%~108%。  相似文献   

3.
合成了3种以4,4’-联吡啶为配体的三核环状Cu(Ⅱ)配合物[Cu3(4,4'-bpy)3.(phen)3](ClO4)6.2H2O(1),[Cu3(4,4'-bpy),(bpy)3](ClO4)6.H2O(2)和[Cu394,4'-bpy)3.(NO2-phen)3](ClO4)6.6H2O(3)。经元素分析,电导,IR,电子光谱,ESR,磁化率等方法进行了表征,推定该配合物具有以4,4’-联吡  相似文献   

4.
方禹之 《分析化学》1998,26(6):694-697
高效毛细管电泳-电化学检测法对6种中国环境优先监测的酚类进行了测定研究,考察了各实验参数对分离、检测的影响。在选定的最佳实验条件下,25 min内基线分离了上述 6种酚类。测得浓度检测限(mg/L):苯酚 0. 01;间-甲酚 0.01;2,4-二氯酚 0.06; 2,4,6-三氯酚0.08;五氯酚0.12;对硝基酚0.07。本方法对实际废水样品中酚的测定结果满意。  相似文献   

5.
研究了反应物配料比3-AMP/Cl(摩尔比)、反应温度与时间对大孔型3-氨甲基吡啶树脂(3—AMPR)性能的影响规律.在最佳合成工艺条件下制得3-AMPR的功能基含量为3.16mmol/g树脂.3-AMPR对AuCl6(2-),PtCl6(2-),IrCl6(2-),PdCl4(2-),RhCl6(3-)的吸附容量分别为800.8,387.8,386.3,133.0,105.5mg金属/g树脂;配位比分别为1.29,0.63,0.64,0.40,0.33。比较了3—AMPR、2-AMPR、4-氨基吡啶树脂(4-APK)、3—APR、2-APR五种树脂对AuCl4-、PtCl6(2-)的吸附性,其中3-AMPR为最佳。  相似文献   

6.
胡顺兴 《大学化学》1994,9(3):33-34
在铵盐存在下,莫尔法滴定时酸度的计算胡顺兴(福建南平师范专科学校福建353000)有存在时,莫尔法的滴定酸度,国内权威教科书上都有明确的示值,pH为6.5~7.2[1-4],但也有的教科书指出,实验证明值的pH为6.0~7.0[5]。经查文献[6],...  相似文献   

7.
在0.06mol/L柠檬酸钠-0.003mol/L HCl(pH6.5)介质中,2,3,4-三羟基-4'-磺基-偶氮苯和铋产生灵敏的单扫描极谱导数峰,铋含量在0~6.7×10^-6mol/L范围内与波高成线性关系,检测限2.4×10^-8mol/L。用提出的方法测定了锡中的铋,并对反应机理进行了研究。  相似文献   

8.
在0.06mol/L柠檬醚钠-0.003mol/LHC1(pH6.5)介质中,2,3,4-三羟基-4′-磺基-偶氮苯和铋产生灵敏的单扫描极谱导数峰,铋含量在0~6.7×10 ̄(-6)mol/L范围内与波高成线性关系,检测限2.4×10 ̄(-8)mol/L。用提出的方法测定了锡中的铋,并对反应机理进行了研究。  相似文献   

9.
林振光  庄鸿辉 《结构化学》1996,15(3):199-204
环己酮与硫代碳酰肼在不同介质中的反应,合成出两个不同的环己烷螺含氮杂环化合物。经X-射线结构分析确定它们分别为1,2,4,5-四氮螺[5,5]十一烷-3-硫酮,C_7H_(14)N_4S(Ⅰ)和1,2,4,-三氮螺[4,5]癸-1-烯-4-氨基-3-硫酮。C_7H_(12)N_4S_x(S_x=0.8S+0.2O)(Ⅱ)。晶体学参数分别为(Ⅰ):P2_1/c,a=12.026(4),b=26.817(6),c=12.042(3),β=115.94(2)°,Z=4,V=933.4(10),M_r=186.28;(Ⅱ):P2_1/m,a=6.595(7),b=6.817(6),c=10.572(6),β=106.3(1)°,V=456(1),Z=2,M_r=181.05。最终一致因子分别为R=0.054,R_w=0.065和R=0.089,R_w=0.096。两个化合物中,环己烷都为椅式构型,它与其螺联的6员氮杂环,5员氮杂环的最小二乘平面间的夹角分别为68.94和90°。并对合成反应途径作了初步讨论。  相似文献   

10.
微分电位溶出法连测血清中铜铅镉锌   总被引:8,自引:1,他引:8  
报道了微分电位溶出法先在0.0025mol.L^-1HCl-0.3mol.L^-1NH4Cl底液中连测血清中Cu、Pb、Cd,再加Ca^3+0.6μg、0.3mlNH4F(2mol.L^-1)于底液,稀释一倍后测Zn。Cu采用标准曲线法,Pb、Cd、Zn采用标准加入法。在选定条件下,四元素的线性关系良好。测试血汪有相对标准偏差≤4.6%,平均回收率为93.3%-101.3%,结果令人满意。  相似文献   

11.
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.
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   

13.
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   

14.
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   

15.
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   

16.
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   

17.
Zhanhui Yang  Shiyi Yang  Jiaxi Xu 《Tetrahedron》2017,73(23):3240-3248
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   

18.
19.
《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   

20.
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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