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1.
本文合成新试剂N-间甲苯基-N′-(氨基对苯磺酸钠)硫脲(MMPT)经红外,紫外,核磁,元素分析等测试,确定其结构,研究测定了试剂与40多种种离子的反应及其配合物的表观洋吸光系数,它可作为Cu^2+(m=0.015μg,c=0.5μg/mL),Ag^+(m=0.1μg,c=3.3μg/mL)的新鉴定试剂和光度法测定Pd^2+(ε309.7=6.32×10^4L.mol^-1.cm^-1,Pt(Ⅳ)  相似文献   

2.
本文研究了meso-四(3,5-二溴-4-羟基苯基)卟啉与铅,锌显色反应的二阶导数光谱行为,建立了同时测定电镀废水中锌和铅的二阶导数光度法。在硼砂-氢氧化钠碱性介质中,沸水浴上加热3min,锌、铅的显色反应即可定量完成。比耳定律范围分别为:0~10μg/25mLZn ̄(2+),0~10μg/25mLPb ̄(2+);检出限为:c_(L、Zn) ̄(2+)=5.6ng/mL,c_(LPb) ̄(2+)=4.0ng/mL。  相似文献   

3.
催化褪色光度法测定痕量钡   总被引:2,自引:0,他引:2  
刘佳铭  马同森 《分析化学》1999,27(10):1215-1218
Ba^2+能在pH5弱酸性介质中催化十二烷基苯磺酸钠(DBS)对铬黑T(EBT0的褪色反应。详细研究了动力学条件,确立测定钡的最适宜催化动力学条件。表观摩尔吸光系数ε620=3.0×10^-6L.mol^-1cm^-1,校正曲线方程为logA0/A=0.006260+0.08704CBa^2+(μg/L);线性范围0-16μg/L(r=0.9991);  相似文献   

4.
新试剂5-氟偶氮胂Ⅰ荧光法测定铝的研究   总被引:2,自引:0,他引:2  
本文报道了新试剂5-氟偶氮胂Ⅰ(5-FAsA-Ⅰ)的合成方法,研究了荧光光度法测定铝的反应条件。Al(Ⅲ)与试剂在pH5.60HAc-NaAc缓冲介质中形成1+1红色配合物并呈现荧光,λex/λem=348.6/391.4nm,线性范围为0~0.2μg/mL,检测限为3.0ng/mL。用于分析茶叶样品中的铝,结果满意。  相似文献   

5.
本文合成新试剂N-间甲苯基-N′-(氨基对苯磺酸钠)硫脲(MMPT),经红外、紫外、核磁、元素分析等测试,确定其结构。研究测定了试剂与40多种离子的反应及其配合物的表观摩尔吸光系数,它可作为Cu2+(m=0.015μg,c=0.5μg/mL)、Ag+(m=0.1μg,c=3.3μg/mL)的新鉴定试剂和光度法测定Pd2+(ε309.7=6.32×104L·mol-1·cm-1)、Pt(Ⅳ)(ε754.4=8.58×104L·mol-1·cm-1)等的显色剂,方法灵敏度高、选择性好,用于阳极泥、人发、矿石及催化剂中上述元素的鉴定或测定,均获满意结果。  相似文献   

6.
本文研究了溴化十二烷基二甲基苄基铵-溴百里酚蓝与阴离子表面活性剂显色反应的适宜条件。结果表明,在pH7.4~8.2范围内阴离子表面活性剂与题示试剂形成1:2:1的绿色离子缔合物,其最大吸收峰位于614nm处。表现摩尔吸光系数分别为:=3.99×10 ̄4L·mol ̄(-1)·cm ̄(-1);=3.70×10 ̄4L·mol ̄(-1)·cm ̄(-1);=1.71×10 ̄4L·mol ̄(-1)·cm ̄(-1)。SDBS在0~195μg/10mL,SDS在0~158μg/10mL,SLS在0~60μg/10mL范围内遵守比耳定律。该法用于河水和生活废水中阴离子表面活性剂测定,结果满意。  相似文献   

7.
桑色素光度法测定痕量铝和聚丙烯酰胺   总被引:2,自引:0,他引:2  
刘佳铭 《分析化学》1999,27(8):972-975
基于聚丙烯酰胺(PAM)作为增稳剂时,Al^3+叠色素(morin)之间的显色反应,提出了一种简便,快速,高灵敏测定痕量铝的光度法,络合物组成比为Al:morin=1:2;表观摩尔吸光系数ε408=6.3×10^7L.mol^-1.cm^-1;铝浓度在0.04-0.28μg/L范围内服从比尔定律;检测限4.0×10^-10g/L。  相似文献   

8.
反相高效液相色谱法同时测定四种氟喹诺酮类药物   总被引:15,自引:0,他引:15  
在SHIM-PACK CLC-ODS柱上,以甲醇与0.05mol/L柠檬酸+0.01mol/L醋酸铵(PH4.5)(V甲醇:V柠檬酸+醋酸铵=25:75)的混合溶液为流动相,要用反相高效相色谱法分离了测定了四种氟喹诺酮类药物;环丙沙星、氧氟沙星、诺氟沙星、依诺沙星,线必不丙沙星和氧氟沙星10~100μg/mL,诺氟沙星和依诺沙星2~80μg/ml,相关系数r〉0.9995,检出限分别为环丙沙星和依  相似文献   

9.
表面活性剂增敏铍试剂Ⅱ荧光法测定痕量锰   总被引:3,自引:0,他引:3  
俞英  黄坚锋 《分析化学》1997,25(5):567-569
在碱性条件下,Mn(Ⅱ)与铍试剂Ⅱ形成1;2的荧光络合物,其荧光峰为λex=λem=367/467(nm),表面活性剂十二烷基苯磺酸钠对体系具有强烈增敏作用,基于此建立了痕量锰的测定方法。本文研究了测定的最佳条件,即0.01%铍试剂Ⅱ4.0mL,0.1mol/LNaOH6.0mL,1%SDBS 4.0mL,反应温度为90℃,时间10min,线性范围为0-160μg/L,回归方程X(μg/L)=2.  相似文献   

10.
烟草中Fe,Co一阶导数分光光度法同时测定的研究   总被引:4,自引:0,他引:4  
本文研究了在pH4.0时,meso-四(4-磺酸基苯基)卟啉与铁、钴同时络合显色的反应条件以及一阶导数光谱行为。此体系一阶导数的灵敏度比零阶导数灵敏度高。Fe ̄(3+)~0.18μg/mL、Co ̄(2+)0~0.24μg/ml,范围内符合比耳定律;检测限为:Fe ̄(3+)=0.48ng/mL,Co ̄(2+)=0.2ng/mL。回收率为:Fe98.5%~100.8%,Co99.2%~101.3%。此方法用于烟草中痕量Fe、Co测定,与AAS值相比较,结果令人满意。  相似文献   

11.
The reaction of malonothioamides with benzene-sulfonyl azide and 2-azido-3-ethylbenzthiazolium tetrafluoroborate gave amides of 2-diazothiomalonic acid, which underwent cyclization to a mixture of 5-N-R-amino-1,2,3-thiadiazole-4-carbothioamides and 5-amino-1,2,3-thiadiazole-4-N-R-carbothioamides. The ratio of the isomeric thiadiazoles formed in this reaction is the same as in the reactions of 2-diazo-2-cyanoacetamides, 5-amino-1,2,3-thiadiazole- and 5-mercapto-1,2,3-triazole-4-carboxamides with P4S10 and of 5-amino-1, 2,3-thiadiazole-4-carbonitriles with H2S; it is characteristic of the influence of substituents on the reactivity of -diazothioacetamides. It was found that the cyclization of the diazo compounds is accelerated when electron-acceptor substituents are attached to the nitrogen atom of the carbothioamide group.Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 8, pp. 1106–1112, August, 1992.  相似文献   

12.
利用手持技术改进测定乙醇分子结构实验   总被引:1,自引:0,他引:1  
利用压强传感器代替排水集气法,改进测定乙醇分子结构实验的仪器装置,并探索最佳反应条件。另外,设计两个空白实验,结合压强变化曲线对实验误差进行相关讨论。  相似文献   

13.
14.
由于石化行业的生产需要,其材质的使用具有多样性和广泛性,经常会出现顾客委托的测试样品的一个或几个元素跨越光谱仪现有测试程序测量范围的情况。本法通过对光谱仪测试原理的认识,根据光谱仪的测试能力及标样的采集,实现了一个或几个元素测量范围的扩展,并对其测量的影响因素进行了研究。  相似文献   

15.
16.
Sets of hydrogen molecule equivalents have been developed which permit the calculation of hydrogenation of different types of carbon-carbon bonds from ab initio total energies (3-21G and 6-31G* basis sets, and, to a more limited extent, for MP2/6-31G* data) of reactants and products. The calculated enthalpies of hydrogenation are in good agreement with experiment for unstrained molecules, with average errors on the order of 2 kcal/mol. The 6-31G* equivalents allow the enthalpies for strained molecules to be calculated accurately, but the 3-21G equivalents do not. The equivalents for both basis sets have been tested by calculating the enthalpies of hydrogenation of carbon-carbon bonds in nitrogen- and oxygen-containing organic molecules, free radicals, and classical carbocations. The results are in good agreement with experiment in most cases.  相似文献   

17.
非那雄胺能抑制5α-还原酶的活性,明显降低二氢睾酮水平,是一种治疗良性前列腺增生的有效药品。该合成工艺以甾烯酮酸为原料,将其与氯化亚砜反应,无须分离即与叔丁胺反应得17β-酰胺化合物,再氧化开环,环合,氢化,脱氢合成了非那雄胺。经元素分析、IR、1HNMR、13CNMR、MS分析表征了其结构。该法无须使用昂贵的2,2-二吡啶二硫化物和剧毒药品苯亚硒酸酐,且以乙酸铵代替氨气,降低了对设备的要求和腐蚀,更适用于工业生产。  相似文献   

18.
实验教学目的是从解决实际问题出发,以实验技术训练和实验设计思想培养为目标。介绍了将单一的物质分配系数测定实验改进为综合实验,提高了实验效果及实验资源利用率。  相似文献   

19.
The compositions of the neutral diterpenoids of the oleoresins of five species of conifers growing in the Transcarpathia have been studied. It has been found that the oleoresins ofAbies alba M.,Larix decidua M., andPicea excelsa L. contain more than 50% of neutral diterpenoids. The group and qualitative compositions of the oxygen-containing diterpenoids have been determined. In the oleoresins ofAbies alba,Picea excelsa, andPicea abies tertiary alcohols — cis-abienol and isocembrol — predominate, while inLarix decidua the main component is the hydroxy ester larixyl acetate. Primary alcohols related to the resin acids have been found in all the oleoresins investigated. Features of the distribution of diterpenoids according to the species of conifers have been revealed. The results obtained are necessary for the chemotaxonomy of conifers of the family Pinceae.  相似文献   

20.
The compositions of the neutral diterpenoids of the oleoresins of five species of conifers growing in the Transcarpathia have been studied. It has been found that the oleoresins ofAbies alba M.,Larix decidua M., andPicea excelsa L. contain more than 50% of neutral diterpenoids. The group and qualitative compositions of the oxygen-containing diterpenoids have been determined. In the oleoresins ofAbies alba,Picea excelsa, andPicea abies tertiary alcohols — cis-abienol and isocembrol — predominate, while inLarix decidua the main component is the hydroxy ester larixyl acetate. Primary alcohols related to the resin acids have been found in all the oleoresins investigated. Features of the distribution of diterpenoids according to the species of conifers have been revealed. The results obtained are necessary for the chemotaxonomy of conifers of the family Pinceae.Novosibirsk Institute of Organic Chemistry, Siberian Branch, Academy of Sciences of the USSR. Translated from Khimiya Prirodynkh Soedinenii, No. 6, pp. 812–816, November–December, 1988.  相似文献   

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