Second derivative spectrophotometric method for simultaneous determination of cobalt, nickel and iron using 2-(5-bromo-2-pyridylazo)-5-diethylaminophenol

A simple, sensitive and rapid derivative spectrophotometric method using 2-(5-bromo-2-pyridylazo)-5-diethylaminophenol (5-Br-PADAP) has been developed for simultaneous determination of Co(II), Ni(II) and Fe(II) which have very similar chemical behavior and appear together in many real samples. The complexes of all these metal ions with 5-Br-PADAP were formed immediately at pH 7.0 ammonium acetate buffered solution and were stable for at least 24 h. Second derivative spectra were selected for evaluation, because working wavelength determination was more precise and spectral overlap was less than in the ordinary and first derivative spectra. Three wavelengths at which the complexes exhibit extremum ²D values for Co(II), Ni(II) and Fe(II) were selected as analytical wavelengths, i.e., 640, 600 and 740 nm, respectively. Calibration curves drawn with zero-to-peak values at mentioned wavelengths were linear between 80 and 2000 ng ml⁻¹ for each metal ion. Concentrations of Co(II) and Ni(II) were calculated from the total ²D values and the sum of the linear equations for these three cations at 640 and 600 nm, after Fe(II) assay by making use of the ²D value at 740 nm. Limits of detection (LOD) for Co(II), Ni(II) and Fe(II) were 2.7, 13.9 and 3.0 ng ml⁻¹, respectively. The method has been applied to tool steel and heater resistance wire samples successfully.     

8-羟基喹哪啶固相萃取光度法测定水样中的铁

研究了8-羟基喹哪啶与铁的显色反应，在pH为8．0的氯化氨-氨水缓冲介质中，在十六烷基三甲基溴化铵(CTMAB)存在下，8-羟基喹哪啶与铁反应生成3：1稳定的蓝紫色络合物，该络合物可被Waters Sep-Park-C18固相萃取小柱萃取，用乙醇洗脱后用光度法测定，络合物λmax=600nm。在此波长下其它金属离子的络合物无光吸收，对铁选择性很好，铁含量在0-5mg/L内符合比尔定律，方法用于水样中痕量铁的测定，结果令人满意。     

痕量Au Bi和Cd的萃取浮选及原子吸收光谱法测定

浮选法分离痕量金属离子,由于灵敏度高、选择性强已得到广泛应用。本文利用浮选法使Au~(3 )、Bi~(3 )和Cd~(2 )同KBr反应生成的络合阴离子与碱性染料罗丹明B(RB)生成既疏水又疏有机溶剂的三元离子缔合物,后者经甲苯浮选分出,用二甲基甲酰胺(DMF)溶解后,可用原子吸收法测定Au、Bi和Cd的含量。本方法用于海水,锌片和矿样中上述三种元素的微量测定,可提高检测灵敏度,而且K、Na、Ca、Mg等共存离子不生干扰。具体实验方法如下:     

新的脉冲进样AAS法测定“麻杏石甘汤”中的微量金属元素

本文研制了一种新的脉冲进样装置，用于火娄原子吸收分光光度法测定中药煎剂中的Ｃａ，Ｍｇ，Ｆｅ，Ｍｎ，Ｚｎ五种金属元素含量，实验表明，利用此种装置可以同时获得两种进样方式的分析结果，线性范围比常规法宽两倍，耗样量，精密度及分析速度均优于常规法。     

紫外分光光度法测定中草药中铁的含量

对白芍、党参、白术、茵陈、天冬、枸杞子、当归、菟丝子、金银花、桔梗中微量元素铁的含量进行了测定,为进一步研究其药理作用提供基础。中草药消化后配制成溶液,用邻二氮菲作显色剂,使用UV-1200型紫外分光光度计在510 nm处测定各样品的吸光度(A),求出样品中微量元素铁的含量。结果显示,当归和金银花中铁的含量较丰富,分别为(135.367 8±0.111 1)μg/g和(125.936 4±0.159 9)μg/g;桔梗含铁量最少,为(3.510 9±0.159 9)μg/g,10种中草药中铁含量有显著性差异(P<0.05)。结果为使用中草药治疗系统疾病提供了可靠数据,10种中草药在用量范围内Fe含量适合人体每天正常摄入量。     

用铜(Ⅱ)-过氧化氢-二苯碳酰二肼/氯仿体系催化-萃取光度法测定铜

本文研究了在弱酸性介质中，利用铜（Ⅱ）催化过氧化氢氧化二苯碳酸二肼生成二苯卡巴腙的指示反应与铜（Ⅱ）和二苯卡巴腙的显色反应相结合，建立了催化-萃取光度法测定铜的新方法。方法的线性范围为5．0～500μg／L，表观摩尔吸光系数为8．8×104L·mol－1·cm-1。用于水、铝合金和岩石中铜的测定。结果满意。     

Flow injection-spectrophotometric determination of cresol compounds in water by reaction withp-aminophenol

A spectrophotometric method has been developed for the simultaneous determination ofo-cresol andm-cresol in water by reaction withp-aminophenol (PAP). Three different methodologies have been assayed; (i) batch analysis, after reaction in an alkaline medium in the presence of dissolved molecular oxygen as oxidizing agent, (ii) a stopped-flow procedure, carried out in the presence of KIO₄ and (iii) a flow injection method based on the same approach. The batch procedure requires 22 min for the full development of colour witho-cresol and 12 min form-cresol. In the stopped-flow mode, using KIO₄ and a reaction time of 12 min, better sensitivity can be obtained for both compounds and limits of detection of 10 g 1^–1 foro-cresol and 30 g 1^–1 form-cresol were found. The flow injection method has a lower sensitivity but permits more than 80 injections per hour. Based on the different maximum absorbance wavelengths obtained for the reaction products of PAP witho-cresol (614 nm) andm-cresol (632 nm), both compounds can be simultaneously determined in water samples and recoveries of 90 to 115% were found in spiked water samples of different types.     

丁基罗丹明B—钼酸盐光度法连续测定铈和钪

在聚乙烯醇（ＰＶＡ）存在下，丁基罗丹明Ｂ（ＢＲＢ）分别与铈钼、钪钼杂多酸络阴离子形成离子缔合物，其最大吸收均位于５７０ｎｍ，表面摩尔吸光度分别为εＣｅ＝３．９６×１０＾６Ｌ．ｍｏｌ＾－１．ｃｍ＾－１，εＳｃ＝４．７１×１０＾５Ｌ．ｍｏｌ＾－１．ｃｍ＾－１，服从比耳定律范围分别为０－２４μｇ／Ｌ Ｃｅ和０－６０μｇ／ＬＳｃ，测定极限为Ｃｅ１．０μｇ／Ｌ（ｎ＝１２）和Ｓｃ１．９μｇ／Ｌ（ｎ＝１０），对     

催化褪色光度法测定痕量钴的研究

研究了在ＰＨ１０．５的Ｎａ２Ｂ４Ｏ７－ＮａＯＨ介质中，痕量钴（Ⅱ）对过氧化氢氧化桑色素初色反应的催化作用，建立了催化动力学光度法测定痕量钴的新方法。方法的线性范围为０－１．２μ／ｍＬ检出限为４．４＊１０＾－１８ｇ／Ｌ。用于水和维生素Ｂ１２中钴的测定，结果满意。     

Synthesis of calix[4]arene library substituted with peptides at the upper rim

A fluorescence-labeled calix[4]arene library substituted with peptides at the upper rim was synthesized. Screening of the library for binding a dye-labeled oligopeptide indicated that some peptidocalix[4]arenes selectively bind the oligopeptide. The chemosensitivity of the library members for a target peptide was also investigated.