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偏最小二乘法辅助分光光度法同时测定痕量锰、铁、铜和锌 总被引:4,自引:0,他引:4
痕量Mn(Ⅱ)、Fe(Ⅲ)、Cu(Ⅱ)和Zn(Ⅱ)与2-(5-溴-2-吡啶偶氮)-5-二乙氨基苯酚和聚乙二醇辛基本基醚在pH8.8发生高灵敏的显色反应,所形成的三元胶束络合物的吸收光谱严重重叠,用偏最小二乘法(PLS)辅助分光光度法成功地同时测定了模拟试样及铝合金和饲料添加剂中上述四种痕量组分。结果表明,PLS法是化学计量学法中一种可适用于基体较复杂的实际试样中痕量组分同时分光光度测定的优良的多元计算方法。 相似文献
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痕量Fe^3+、Mn^2+、Cu^2+、Zn^2+与2-(5-溴-2-吡啶偶氮).5-二乙氨基苯酚(5-Br-PADAP)和对.(1,1,3,3.四甲基丁基)苯基醚(Triton X-100)在pH8.3发生高灵敏显色反应,所形成的三元胶束络合物的吸收光谱严重重叠。本文采用主成分-偏最小二乘法(PC—PLS)辅助分光光度法成功地测定了合成试样及饲料中上述4种痕量组分。结果表明,PC—PLS法是化学计量学法中一种可适用于基体较复杂的实际试样中痕量组分同时分光光度测定的优良的多元计算方法。 相似文献
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偏最小二乘法辅助分光光度法同时测定痕量锰,铁铜和锌 总被引:4,自引:0,他引:4
痕量Mn(Ⅱ),Fe(Ⅲ),Cu(Ⅱ)和Zn(Ⅱ)与2-(5-溴-2-吡啶偶氮)-5-二乙氨基苯酚和聚乙二醉辛基苯基醚在ph8.8发生高灵敏的显色反应,所形成的三元胶束络合物的吸收光谱严重重叠,用偏最小二乘法(PLS)辅助分光光度法成功地同时测定了模拟试样及铝合金和饲料添加剂中上述四各痕量组分,结果表明,PLS法是化学计量学法中一种可适用于式体较复杂的实际试样中痕量组分同时分光光度测定的优良的多元 相似文献
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混合线性分析-分光光度法同时测定微量锌、镉、汞 总被引:11,自引:0,他引:11
提出了以2-(5-溴-2-吡啶偶氮)-5-二乙氨基酚为显色剂分光光度法同时测定锌、镉、汞的新方法。由于在可见区3种络合物的吸收光谱具有相似的特征和严重重叠,本文采用混合线性分析进行光谱分辨,各组分的纯光谱则用最小二乘法从校正集中求出。讨论了显色条件,波长选择,纯光谱的确定和吸光度加合性等因素对测定的影响。方法具有简单,快速,准确等优点。已成功地应用于混合试样中锌、镉、汞的同时测定,并与同条件下偏最小二乘法的计算结果进行了对比。 相似文献
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二溴对甲基偶氮羧催化动力学光度法测定痕量铜 总被引:6,自引:0,他引:6
1引言目前催化动力学光度法测定痕量元素已有不少报道,但极少见利用不对称偶氮羧类试剂进行催化动力学测定的文献。二溴对甲基偶氮羧是一种新的显色剂,本文研究发现其在HAc-NaAc介质中,以a,a’-联吡啶为活化剂,痕量钢能强烈催化抗坏血酸还原二溴对甲基偶氮羧的反应,其反应速度与铜的浓度符合动力学一级反应关系,检出限为4.6×10-11g/mL,可用于测定食品及饮用水中的痕量铜。2实验部分2.1仪器与试剂751型分光光度计(上海分析仪器厂)。0.1mg/LCu(Ⅱ)标准溶液(按常规法配制);1g/LM… 相似文献
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在pH5.3的HAc-NaAc、2-(3,5-二溴-2-吡啶偶氮)-5-二乙氨基酚(3,5-Br2-PADAP)、溴代十六烷基三甲铵(CTMAB)溶液中,用线性扫描示波极谱法可得到锑(Ⅲ)的络合物吸附波。峰电位为-0.70V(vs.SCE)。二阶导数档峰高与Sb(Ⅲ)浓度在3.3X10-8~2.5X10-6mol/L范围内呈线性关系。检出限为8.2X10-9mol/L。用多种电化学方法研究了极谱波的性质及电极反应机理。络合物组成为Sb(Ⅲ):3,5-Br2-PADAP=1∶2。加入CTMAB可消除试剂峰且提高灵敏度。试验了30多种离子对峰电流的影响,用流基棉分离干扰离子。方法已用于矿样中锑的测定。 相似文献
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小波变换-偏最小二乘法用于钨、钼、钛的分光光度法同时测定 总被引:13,自引:0,他引:13
1引言小波分析方法是一种新发展起来的数学方法。本文采用小波分析光谱实验数据进行预处理,然后用偏最小二乘法(PLS)进行校正,完成了钨、钼、钛的同时测定。2实验部分2.1主要仪器与试剂日立557双波长分光光度计;奔腾586微机。W(Ⅵ)标准溶液10mg/L;Mo(Ⅵ)标准溶液2mg/L;Ti(Ⅳ)标准溶液2mg/L;水杨基荧光酮(SAF)1.0×10-3mol/L;溴化十六烷基三甲铵(CTMAB)5×10-3mol/L。2.2实验步骤(1)取一定量的W、Mo、Ti标准溶液于25mL比色管中,依次加入2mL5mol/LHCl,2,5mLSAF溶液,4.0mL(::FNIn,然看… 相似文献
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以2-溴乙醇作重原子微扰剂,用亚硫酸钠化学除氧技术,建立了β-环糊精诱导室温磷光法(β-CD-RTP)测定痕量二氢苊,芴,菲,7,8-苯并喹啉的方法。该法除氧简便快速,体系澄清。 相似文献
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Kristýna Urbánková Martin Moos Jiří Machát 《International journal of environmental analytical chemistry》2013,93(11):1077-1087
This paper deals with a simplified multi-element profiling of inorganic arsenic, antimony, selenium and tellurium in the form of 75As, 82Se, 121Sb and 125Te by ICP-MS for amounts less than 10?µg?L?1. Internal standards such as 72Ge and 209Bi were successfully used for the suppression of both influence of macro elements Na+, K+, Ca2+, Mg2+ or Al3+, and interference of limited concentrations of heavy metal ions. Modified silica sorbents Separon? SGX C18, C8, CN, NH2, RPS and Phenyl were tested for the preconcentration of As, Sb, Se and Te (0.25–5?µg?L?1) in the form of ion associates with cationic surfactants from 50–250?mL sample volume. 1-etoxycarbonyl-pentadecyltrimethylammonium bromide (Septonex®, 0.005?mol?L?1) was suitable for this purpose in the presence of 4-(2-pyridylazo) resorcinol, 2-pyrrolidinecarbodithioate and 8-hydroxyquinoline-5-sulphonic acid. The quantitative retention occurred at pH 7?±?0.2 and the mixture of acetone with ethanol in ratio 1?:?1 in the presence of 0.1?mol?L?1 HCl was used for the quantitative elution. Organic solvents and the excess of acid were removed by evaporation prior to the determination by ICP-MS. The determination of the above trace metalloids in various kinds of water with enrichment factor till 50 times on silica Separon? SGX C18 and the above reagents were compared with the standard addition method. 相似文献
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K. Elaine Hubbard Amy Wells Thandranese S. Owens Michael Tagen Charles H. Fraga Clinton F. Stewart 《Biomedical chromatography : BMC》2010,24(6):626-631
A method to rapidly measure dopamine (DA), dihydroxyindolphenylacetic acid, homovanillic acid, serotonin (5‐HT) and 5‐hydroxyindoleacetic acid concentrations in cerebrospinal fluid (CSF) has not yet been reported. A rapid, sensitive, and specific HPLC method was therefore developed using electrochemical detection. CSF was mixed with an antioxidant solution prior to freezing to prevent neurotransmitter degradation. Separation of the five analytes was obtained on an ESA MD‐150 × 3.2 mm column with a flow rate of 0.37 mL/min and an acetonitrile–aqueous (5 : 95, v/v) mobile phase with 75 mM monobasic sodium phosphate buffer, 0.5 mM EDTA, 0.81 mM sodium octylsulfonate and 5% tetrahydrofuran. The optimal electrical potential settings were: guard cell +325 mV, E1 ?100 mV and E2 +300 mV. Within‐day and between‐day precisions were <10% for all analytes and accuracies ranged from 91.0 to 106.7%. DA, 5‐HT, and their metabolites were stable in CSF with antioxidant solution at 4°C for 8 h in the autoinjector. This method was used to measure neurotransmitters in CSF obtained from children enrolled on an institutional medulloblastoma treatment protocol. Copyright © 2009 John Wiley & Sons, Ltd. 相似文献
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Synthesis,Persistent Luminescence,and Thermoluminescence Properties of Yellow Sr3SiO5:Eu2+,RE3+ (RE=Ce,Nd, Dy,Ho, Er,Tm, Yb) and Orange‐Red Sr3−xBaxSiO5:Eu2+, Dy3+ Phosphor 下载免费PDF全文
Dr. Ye Li Baohong Li Chenchen Ni Shuxia Yuan Jing Wang Prof. Qiang Tang Prof. Qiang Su 《化学:亚洲杂志》2014,9(2):494-499
Sunlight‐excitable orange or red persistent oxide phosphors with excellent performance are still in great need. Herein, an intense orange‐red Sr3?xBaxSiO5:Eu2+,Dy3+ persistent luminescence phosphor was successfully developed by a two‐step design strategy. The XRD patterns, photoluminescence excitation and emission spectra, and the thermoluminescence spectra were investigated in detail. By adding non‐equivalent trivalent rare earth co‐dopants to introduce foreign trapping centers, the persistent luminescence performance of Eu2+ in Sr3SiO5 was significantly modified. The yellow persistent emission intensity of Eu2+ was greatly enhanced by a factor of 4.5 in Sr3SiO5:Eu2+,Nd3+ compared with the previously reported Sr3SiO5:Eu2+, Dy3+. Furthermore, Sr ions were replaced with equivalent Ba to give Sr3?xBaxSiO5:Eu2+,Dy3+ phosphor, which shows yellow‐to‐orange‐red tunable persistent emissions from λ=570 to 591 nm as x is increased from 0 to 0.6. Additionally, the persistent emission intensity of Eu2+ is significantly improved by a factor of 2.7 in Sr3?xBaxSiO5:Eu2+,Dy3+ (x=0.2) compared with Sr3SiO5:Eu2+,Dy3+. A possible mechanism for enhanced and tunable persistent luminescence behavior of Eu2+ in Sr3?xBaxSiO5:Eu2+,RE3+ (RE=rare earth) is also proposed and discussed. 相似文献
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Recai İnam Tuba Sarİgül Ebru Zeynep Gülerman NazlI Uncu 《International journal of environmental analytical chemistry》2013,93(15):1135-1149
A novel, sensitive, simple, fast, and fully validated differential pulse polarographic (DPP) method for the determination of trace amounts of thifensulfuron-methyl in pesticide formulation, soil, and orange juice is reported. This procedure was based on a highly sensitive peak formed due to the reduction of thifensulfuron-methyl on a dropping mercury electrode over the pH range 1.00–10.00 in Britton–Robinson buffer. The polarographic reduction exhibits only a single peak in the pH ranges pH?≥?3.0 and pH?≤?6.0 and pH?=?10.0 located at potential values of ?1.010, ?1.350, and ?1.610?V (vs. SCE), respectively. The single peak appeared as a maximum at pH 3.0 (?1.010?V) was well resolved and suitable to be investigated for analytical use. This peak showed quantitative increments with the additions of standard thifensulfuron-methyl solution under the optimal conditions, and the cathodic peak current was linearity proportional to the thifensulfuron-methyl concentration in the range of 2?×?10?7–5?×?10?5?M. The limit of detection (LOD) and limit of quantification (LOQ) were obtained as 1.05?×?10?7 and 3.50?×?10?7?M, respectively, according to the relation k ?×?SD/b (where k?=?3 for LOD, k?=?10 for LOQ, SD is the standard deviation of the blank, and b is the slope of the calibration curve). The proposed method was applied to pesticide formulation (Harmony® Extra), and the average percentage recovery was in agreement with that obtained by the spectrophotometric comparison method, 97.82 and 102.6%, respectively. The method was extended to determination of thifensulfuron-methy in spiked soil and orange juice, showing a good reproducibility and accuracy with a relative standard deviation of 4.55 and 1.40%, and relative errors of +2.80 and +1.90%, respectively. 相似文献
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Energetic and structural characteristics of new sandwich compounds of the second row elements X(Y3)2 and X(Y4)2 (X = B5?, C4?, N3?, O2?, Y = C, Si) stabilized with lithium cations were investigated using the methods of density functional theory B3LYP/6-311+G(d,p) and ab initio MP2(full)/6-311+G(d,p). Carbon sandwich systems were found to be thermodynamically more stable than their silicon analogs. In all systems the formation of hypercoordinated central atom is observed. For the most representative structures the Bader topological analysis of electron density was performed. The key types of distortions in the silicon-containing systems were found. 相似文献
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采用溶胶-凝胶法制备系列的镁掺杂Y2-xMgxRu2O7-δ(YMRO?x,x=0.05、0.1、0.15)催化剂,通过X射线光电子能谱对其进行价态分析发现,采用小离子半径的Mg^2+取代烧绿石结构中处于A位的部分Y^3+,进一步增加了烧绿石结构中氧缺陷数量,也引发了部分Ru^4+转变为Ru^5+,释放电子到表面,促进了氧析出反应(OER)。其中YMRO?0.1催化剂的含氧缺陷浓度最高,其催化活性最高。在达到10 mA·cm^-2电流密度时,相比于RuO2(358 mV)、Y2Ru2O7-δ(294 mV),YMRO?0.1仅需施加265 mV过电位并且其Tafel斜率相对于RuO2(88 mV·dec^-1)和Y2Ru2O7-δ(64 mV·dec^-1)仅为45 mV·dec^-1。此外,由于氧空位增多,即活性位点增多,降低了自由基从金属位点脱附的吉布斯自由能,促进了OER催化性能。第一性原理表明,替位原子MgY与氧空位形成复合体,可以降低氧空位形成能,同时随着Mg^2+引入,带隙变小,电荷迁移能也随之变小,进而可以得到更高的催化活性。 相似文献
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Fe(II) induces the reaction between Tl3+ and H2O2. The rate of reaction is linearly proportional to the concentration of Fe2+ in the range 2.5 ?10-9-2.5 ?10-8 mol dm-3 (20? and 5 ?10-9-5 ?10-8 mol dm-3 (15?. The standard deviation is less than 0.071 ?10-8. A 1000-fold excess of Zn2+, Cd2+, Mg2+, Ni2+, Pb2+, Ba2+, Ca2+, Li+, Na+, Ag+, NO3-, SO42-, AcO-, HPO42-, 500-fold excess of Al3+, Fe3+, Co2+, Hg2+ and 100-fold excess of Ti4+, Cr3+, Cu2+, Br-, Cl- can be tolerated, but reducing agents such as (NH2)2SO4, NH2OH.HCl interfered. This kinetic method was applied to determine Fe(II) in standard zinc sample and fountain water, with satisfactory results. 相似文献
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Mehrorang Ghaedi Morteza Montazerozohori Arash Hekmati Mostafa Roosta 《International journal of environmental analytical chemistry》2013,93(8):843-857
Trace amounts of Fe3+, Pb2+, Cu2+, Ni2+, Co2+ and Zn2+ ions were efficiently enriched following complexation with silica-gel chemically functionalized with 2-((3-silylpropylimino)methyl)-5-bromophenol. The enriched metal ions efficiently eluted with 6?mL of 4.0?mol?L?1 nitric acid and their metal contents were determined by flame atomic absorption spectrometry (FAAS). The influences of the analytical parameters and experimental variables on the recoveries of the metal ions under study were investigated and optimized. The method has high sorption preconcentration efficiency even in the presence of various interfering ions. At optimum values of all variables the method is applicable for analysis of real samples with recoveries in the range of 95 to 105% with RSD lower than 4.2% and detection limits between 1.4 and 2.8?µg?L?1. 相似文献
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Antibacterial activity of transition metal complexes with a tridentate NNO amoxicillin derived Schiff base. Synthesis and characterization 下载免费PDF全文
From the reaction of amoxicillin ( 1 ) antibiotic with 2,6?diaminopyridine ( 2 ) an amoxicillin?based Schiff base (HL) ( 3 ) was obtained and its transition metal Schiff base complexes were synthesized. Spectroscopic and physicochemical techniques, namely, UV?Vis, FT?IR, 1H?NMR, EPR, mass spectrometry, molar conductance, magnetic susceptibility, molecular modelling, together with elemental and thermal analyses, were used to characterize the synthesized compounds. Spectral and magnetic data suggested an octahedral geometry for all the complexes and the general formulae [ML(H2O)3][PF6] (M(II) = Mn2+ ( 4 ), Co2+ ( 5 ), Ni2+ ( 6 ), Cu2+ ( 7 ), Zn2+ ( 8 ), was proposed for them, where L represents deprotonated tridentate NNO amoxycillin?derived Schiff base. All compounds were screened for antibacterial activity by using agar disc diffusion method. The zinc(II) complex exhibited promising bactericidal activity against E. coli and S. aureus. 相似文献