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1.
2-(5-溴-2-吡啶偶氮)-5-二乙氨基苯酚(5-Br-PADAP)在极谱和伏安分析中的应用已有一些报道。陈林林等曾经研究过Ti(Ⅳ)-5-Br-PADAP络合物在稀H2SO4-H2C2O4溶液中的极谱行为,但灵敏度不高(1.0×10-7mol/L)。我们发现,在pH4.1左右的HAc-NaAc底液中,Ti(Ⅳ)-5-Br-PADAP-NaClO3体系产生一灵敏的极谱吸附催化波,二次导数峰电位在-0.86V(vs.SCE)左右,波形良好,波高稳定,检测限可达4×10-10mol/L。1 实验部…  相似文献   

2.
流动注射化学发光同时测定废水中的三价铬和六价铬   总被引:14,自引:4,他引:10  
张海松  杨秀岑 《分析化学》1995,23(10):1148-1150
首次将镀铜锌粒作成优良的还原柱,在线还原Cr(Ⅵ)成Cr(Ⅲ),以鲁米诺-H2O2(KBr)体系流动注射化学发光同时测定废水中两种价态的铬。分析速率为60试样/h;线性范围为1.0×10^-5-1.0×10^-9mol/L;测Cr(Ⅲ)及Cr(Ⅵ)的相对标准偏差(n=6)分别为0.37%-4.0%及1.2%-4.4%;测定Cr(Ⅲ)的检出限2.3×10^-11mol/L。测定结果与标准方法无显差  相似文献   

3.
脱氧核糖核酸变性和损伤的吸附伏安法研究   总被引:2,自引:0,他引:2  
陆宗鹏  卢莠芬 《分析化学》1996,24(4):463-466
本文用汞电极(HMDE)二次导数阴极吸附伏安(SD-AdCSV)和碳电极(GCE、CPE)导数循环伏安(FD-CV)法研究了核酸受热、紫外线、超声波和丝裂霉素C(MMC)作用下的变性作用。在0.1mol/L(K2HPO4+KH2PO4)-0.1mol.L NaCl(pH7.0)底液中,吸附的单股(ss-)和双螺旋(ds-)DNA分别在HMDE上得到特征还原峰P3和P2,和在碳电极上得到氧化峰A。物  相似文献   

4.
肿瘤细胞中长春新碱的高效液相色谱法测定   总被引:10,自引:0,他引:10  
黎丹戎  涂文升  李力  唐东平  黄薇 《色谱》1998,16(1):50-52
 长春新碱(VCR)为重要和常用抗肿瘤药物之一。肿瘤细胞耐药性是导致化疗失败的主要原因。为了筛选耐药细胞的逆转剂,建立了测定肿瘤细胞内VCR浓度的高效液相色谱法,色谱条件为:Zorbax-ODS反相柱25cm×4.6mmi.d.,流动相:0.02mol/LK2HPO4(pH6.6)∶CH3OH(20∶80,V/V),流速:1.0mL/min,检测波长:267nm。方法简单、快速、选择性好,在10~200mg/L范围内VCR浓度-峰高呈良好的线性关系(r=0.9998),仪器灵敏度为4ng。  相似文献   

5.
硼掺杂多晶金刚石薄膜电极的电化学特性   总被引:1,自引:0,他引:1  
朱建中  许春芳 《分析化学》1995,23(7):824-827
用循环伏安法和恒电位法研究了硼掺杂多晶金刚石薄膜电极(DFE)的若干电化学特性。电极面积4×4mm^2。在0.1mol/L KCl,NaNO3,NaOH和KH2PO4+Na2HPO4(pH=6.86)电解质溶液中电势窗口均为-500 ̄+800mV;而在0.1mol/L HCl和H2SO4溶液中电势窗口为-200 ̄+1100mV.K3Fe(CN)6的氧化峰电位为+500mV,与Pt电极测量相同;校正  相似文献   

6.
KBrO3—KBr紫外分光光度法测定痕量水杨酸   总被引:5,自引:0,他引:5  
研究了HCl溶液中KBrO3-KBr紫外分光光度法测定水杨酸的条件,建立了测定痕量水杨酸的新方法。结果表明,在0.6mol/LHCl,3*10^-5mol/LKBrO3,5*10^-4mol/LKBr,6*10^-4mol/lKI溶中测定水杨酸,其线性范围为0.2-4.0mg/L,表观摩尔吸光系数为1.9*10^-4L.mol^-1.cm^-1,Sandell为7.3μg/cm^2。sg if e  相似文献   

7.
本文比较了Mo(Ⅵ)-1-(2-吡啶基偶氮)-2-萘酚(PAN)与Mo(Ⅵ)-4(2-吡啶基偶氮)间苯二酚(PAR)的极谱性质,讨论它们在作为吸附波试剂时的优缺点,以求得在选择络合剂时的感性和理性认识.本文还报道了Mo(Ⅵ)-PAN-KBrO3吸附催化波体系,最佳实验条件,0.1mol/LHAc--NaAc,pH=4.6,0.01mol/LKBrO3,2.5×10-5mol/LPAN.峰电位为-0.71V(vs.SCE),检出限1×10-9mol/L,线性范围0~6×10-7mol/L  相似文献   

8.
邹永明  丁中涛 《分析化学》1994,22(11):1115-1117
Cr(Ⅵ)在NH4OH-NH4Cl-NaNO2-8-氨基喹啉-5-偶氮-对苯磺酸钠体系中产生一灵敏的阴极极化二次导数催化波,其峰电位在-1.33V(vs.SCE)。Cr(Ⅵ)在0.40 ̄12.0ng/ml范围内与峰电流成正比。本法已用于为水中Cr(Ⅵ)的测定,结果良好。  相似文献   

9.
原子吸收法测定环境水样中化学需氧量   总被引:9,自引:3,他引:6  
在H2SO4介质中用K2Cr2O7同COD水样反应,反应后水相中过量的Cr(Ⅵ)以Cr2O2-7形式被TOA萃入有机相中,而生成的Cr(Ⅲ)则留在水相,用AAS测定有机相中的Cr(Ⅵ)或水相中的Cr(Ⅲ)都可求得COD含量。本法简便快速、需样量少、且测定结果同标准方法(CODCr法)一致,回收率为98%~108%,平均标准偏差为3.3%。  相似文献   

10.
示波极谱测定天然水,食品和生物样品中痕量锡   总被引:1,自引:0,他引:1  
在H2SO4-HClO4-NaBr-(NH4)2VO3的体系中,Sn(Ⅳ)在-0.60V左右产生一个非常灵敏的极谱催化谱,Sn(Ⅳ)浓度在0.8-160ng.mL^-1之间与峰电流成线性关系,检测限为0.26ng.mL^-1。该法应用于天然水、食品和生物样品中痕量锡的测定,结果令人满意。  相似文献   

11.
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   

12.
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   

13.
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   

14.
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   

15.
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   

16.
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   

17.
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   

18.
An efficient approach to the synthesis of highly congested di, penta and hexacyclic pyrazoles as well as imidazole fragment containing novel heterocyclic molecule has been developed through a carbanion induced transformation of suitably functionalized 2H-pyran-2-ones, benzo[h]chromene and thiochromeno[4,3-b]pyrans. Due to the presence of fluorescence, we report their prime application metal sensor as off/on switching in ferric ions.  相似文献   

19.
20.
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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