2,3,7-三羟基-9-(4,5-二溴-邻硝基)苯基荧光酮与钨(Ⅵ)的显色反应研究

研究了在阳离子表面活性剂溴化十六烷基三甲铵(CTMAB)存在下,2,3,7 三羟基 9 (4,5 二溴 邻硝基)苯基荧光酮(DBONPF)与钨(Ⅵ)的显色反应及光度性能。在0.4mol LH2SO4介质中,试剂与钨(Ⅵ)形成化学计量比为2∶1的红色络合物,其最大吸收峰位于547nm波长处,表观摩尔吸光系数为5.64×105L·mol-1·cm-1,检出限为4.12μg L,钨质量浓度在0～500μg L范围内符合比尔定律,分析方法可用于钢样中微量钨的测定。     

2,3,7-三羟基-9-(2-羟基)萘基荧光酮光度法测定环境样品中微量铬(Ⅵ)

研究了在阳离子表面活性剂溴化十六烷基三甲胺(CTMAB)存在下,有机显色试剂2,3,7-三羟基-9-(2-羟基)萘基荧光酮(2-HNF)与Cr(Ⅵ)的显色反应和光度性质。结果表明,在pH=7.30的Na2HPO4-KH2PO4缓冲介质中,30min内可反应完全,2-HNF与Cr(Ⅵ)形成摩尔比为2∶1的紫红色络合物,络合物至少能稳定存在12h,其最大吸收波长位于570nm处,表观摩尔吸光系数为1.07×105L·mol-1·cm-1,Cr(Ⅵ)含量在0～1.40μg/5mL范围内符合比耳定律。该分析方法已用于环境样品中微量铬的测定,结果满意。     

2,3,7-三羟基-9-(2-羟基-5-对甲苯偶氮)苯基荧光酮应用于中草药中痕量锗的测定

研究了新试剂2,3,7-三羟基-9-(2-羟基-5-对甲苯偶氮)苯基荧光酮(THH-p-MPAPF)与锗(Ⅳ)的显色反应,建立了测定中草药中痕量锗的光度分析方法。在6.0 mol/L H3PO4介质中,THH-p-MPAP与锗(Ⅳ)反应生成红色配合物,配合物最大吸收峰位于501 nm,表观摩尔吸光系数达2.1×105L.mol-1.cm-1,锗量在0~0.72μg/mL符合比尔定律。该显色反应体系具有非常好的选择性和稳定性,在不加任何掩蔽剂的情况下,金属离子允许量大多在10 mg以上,尤其是大量钼和钨不干扰锗测定,方法选择性明显优于其他同类试剂,已用于某些中草药中锗的测定。     

2,3,7-三羟基-9-水杨基荧光酮分光光度法测定痕量铌

以酒石酸作为辅助络合剂,在表面活性剂溴化十六烷基吡啶存在下及pH 5.5的乙酸-乙酸钠缓冲溶液中,显色剂2,3,7-三羟基-9-水杨基荧光酮与铌(Ⅴ)形成稳定络合物,其最大吸收波长位于560nm处,据此提出了分光光度法测定铌钽矿浸出液中铌含量的方法。铌(Ⅴ)的质量浓度在4～240μg·L-1范围内符合比耳定律,表观摩尔吸光率为1.44×106L·mol-1.cm-1。方法用于铌钽矿样品中痕量铌的测定,测定结果与国家标准方法测定值相一致。     

胶束增敏 2,3,7-三羟基-9-[3,5-二溴-4-(2,5-二羟基)苯偶氮]苯基荧光酮与锆(Ⅳ)显色反应的研究

系统研究了在混合表面活性剂 CTMAB-Tween-80 存在下,新显色剂 2,3,7-三羟基-9-[3,5-二溴-4-(2,5-二羟基)苯偶氮]苯基荧光酮(DBAPPF) 与 Zr(Ⅳ)的显色反应及其光度性质并讨论了混合表面活性剂对显色反应的增敏机理.在浓度为 0.4mol/L 的 HCl 介质中,新试剂与 Zr(Ⅳ)和表面活性剂形成胶束络合物,混合表面活性剂有较强的增敏作用,络合物最大吸收波长为 539 nm,表观摩尔吸光系数为 1.55×105 L·mol-1·cm-1.锆(Ⅳ)的质量浓度在 0～0.32 mg/L 范围内服从比尔定律.方法已用于铝合金中微量锆的测定.     

2,3,7-三羟基-9-(2,4-二羟基)苯基荧光酮荧光猝灭法测定锰(Ⅱ)

在pH=9.33的NH3.H2O-NH4Cl缓冲介质中,于表面活性剂溴化十六烷基三甲铵(CTMAB)存在下,利用Mn(Ⅱ)与2,3,7-三羟基-9-(2,4-二羟基)苯基荧光酮(DHPF)形成Mn(Ⅱ)-DHPF-CTMAB三元配合物可产生荧光猝灭,建立了荧光猝灭法测定痕量Mn(Ⅱ)的新方法。该体系激发波长λex=520nm,发射波长λem=540nm,荧光猝灭值与Mn(Ⅱ)的含量在0～0.36μg/25mL范围内呈线性关系,检出限为0.02μg/25mL,在CTMAB存在下,配合物摩尔比Mn(Ⅱ)∶DHPF=1∶2。拟定方法用于测定尿样中微量锰的含量,结果满意。     

新型显色剂2,3,7-三羟基-9-(3,5-二氯-4-羟基)苯基荧光酮与钨(Ⅵ)的显色反应

研究了在阳离子表面活性剂溴化十六烷基三甲胺(CTMAB)存在下 ,新试剂2,3,7_三羟基_9_(3,5_二氯_4_羟基)苯基荧光酮(DCHPF)与钨(Ⅵ)的显色反应及光度性能 ;在0.6mol/LHCl介质中 ,试剂与钨(Ⅵ)形成化学计量比为2∶1的红色络合物 ,其最大吸收峰位于536nm波长处 ,表观摩尔吸光系数为1.28×105L·mol-1·cm-1,钨含量在0～0.4mg/L范围符合比尔定律 ;拟定分析方法用于钢样中微量钨的测定 ,结果令人满意。     

2-羟基-3-甲氧基苯基荧光酮分光光度法测定中药中痕量锗

研究了新试剂2羟基3甲氧基苯基荧光酮(HMPF)与锗的显色反应。建立了测定几种中药中锗的光度分析方法。在磷酸(2+1)介质和非离子型表面活性剂OP介质中,2羟基3甲氧基苯基荧光酮与锗发生灵敏的显色反应,其最大吸收峰为505.50nm,表观摩尔吸光系数为1.56×105L·mol-1·cm-1,锗量在0～12μg/25mL符合比耳定律。锗与试剂的显色反应有良好的选择性,绝大多数金属离子特别是钙、镁、铁、锌和钼有非常高的允许量,可直接应用于几种中药中锗的测定,结果满意。     

2,3,7-三羟基-9-[3,5-二溴-4-(2,4-二羟基)苯偶氮]苯基荧光酮的合成及与锆(Ⅵ)的显色反应

介绍了新试剂2,3,7三羟基-9-[3,5-二溴-4-（2,4二羟基）苯偶氮]苯基荧光酮（DBARPF）的合成。通过元素分析、红外光谱和紫外光谱等方法测试,确定了该试剂的组成和结构。研究了试剂与一些金属离子显色反应的光度性质,建立了光度法测定微量锆（Ⅳ）的新方法。在0．6mol/L盐酸介质中,阳离子表面活性剂CTMAB存在下,锆（Ⅳ）与DBARP形成稳定的1：4水溶性络合物,λmax＝538nm,λ538nm为1．78×105L·mol-1·cm-1。锆（Ⅳ）含量在0～400μg/L范围服从比尔定律。拟定方法用于铝合金样品中微量锆（Ⅳ）的测定,获得满意的结果。     

二甲氧基羟基苯基荧光酮光度法测药物中的钼

钼是维持人体健康的重要微量元素之一,主要作用是防止龋齿,促进铁的新陈代谢,保持男子的性能力,预防贫血,尤其具有抗癌防癌等生物学效应。钼缺乏与很多疾病有关,尤其是动脉粥样硬化的致病因素。为了保持人体健康,就要保证微量元素钼的正常摄入量。世界卫生组织估     

Spectrophotometric determination of zirconium with 9-methyl-2,3,7-trihydroxy-6-fluorone

Summary 9-Methyl-2.3.7-trihydroxy-6-fluorone has been used as a new colorimetric reagent for zirconium. The rose-red complex shows maximum absorption, against the reagent blank, at 500 nm and obeys Beer's law from 0.1 to 2.5 ppm. The optimum concentration range is from 0.66 to 2.5 ppm, where the per cent relative analysis error is 2.96. The composition of the complex, obtained from Job's method, indicates that the complex in solution contains the metal and the reagent in a ratio of 11. The instability constant of the complex is 1.07 · 10^–6.     

Spectrophotometric determination of molybdenum with 9-methyl-2,3,7-trihydroxy-6-fluorone

9-Methyl-2,3,7-trihydroxy-6-fluorone is proposed as a highly sensitive reagent for molybdenum. Thc rose-red complex shows maximum absorption at 510 mμ and obeys Beer's law from 0.2 to 3 p.p.m. of molybdenum, the optimum range being 08 to 3 p p m. where the percent relative analysis error is only 28. In solution the complex contains molybdenum and the reagent in the ratio 1:1. The instability constant of the complex is about 2.09·10^-6.     

Spectrophotometric determination of molybdenum with phenylfluorone

Spectrophotometric studies on the reaction between molybdenum as molybdate (MoO₄^2?) and phenylfluorone are presented. The reaction conditions are optimized to develop an intense color (molar absorptivity is 3.8 × 10³) selective and sensitive for the Spectrophotometric determination of molybdenum. The absorbance is measured at 560 nm, at a pH of 1.5–3. The colored complex is stable for up to 24 hr, Beer's law is obeyed, over the concentration range of 1 to 4 μg/25 ml. The relative standard deviation is 2% and the sensitivity of the method is 1.60 × 10^?4 mg/ml.     

Spectrophotometric determination of iron(III)-dimethyldithiocarbamate (ferbam) using 9-(4-carboxyphenyl)-2,3,7-trihydroxyl-6-fluorone

A spectrophotometric method was developed for the determination of iron(III)-dimethyldithiocarbamate (ferbam) by concerting it into an iron(III)-9-(4-carboxyphenyl)-2,3,7-trihydroxyl-6-fluorone complex. In NH₃-HAc buffer solution (pH 6.5), the reagent reacts with ferbam to form a blue complex with a maximum absorption peak at 640 nm. The reaction can be completed rapidly at room temperature and the absorbance is stable for at least 24 h. The apparent molar absorption coefficient, Sandell’s sensitivity of the complex, the detection limit and the relative standard deviation were found to be 1.06×10⁵ l mol⁻¹ cm⁻¹, 3.9 ng cm⁻², 2.2 ng ml⁻¹ and 1.06%, respectively. From 0 to 75 μg of ferbam in 25 ml solution the absorbance obeyed Beer’s law. The effect of foreign ions and other dithiocarbamates were also studied in detail. The results indicated that all coexisting ions examined can be tolerated in considerable amounts, especially other dithiocarbamates such as ziram and zineb, which always interfere with the determination of ferbam in the literature. The proposed method is very sensitive, selective and simple, it has been applied to determine ferbam in commercial samples.     

Spectrophotometric determination of chromium(VI) through ion-pair formation with phenylfluorone

Two successive outer sphere complexes with mole ratios of 1:1 and 1:2 are formed between chromium(VI) and phenylfluorone at pH 1.5 in 40% ethanol. These have absorption maxima at 490 and 470 nm, respectively. The 1:1 complex obeys Beer's law at 500 nm (? = 2.1 × 10⁴ 1 mol^-1 cm^-1) in the range 13–1700 ng l^-1 chromium(VI).     

2, 3, 7-三羟基-9-间羟基苯基荧光酮的合成及其 分析性能的研究

研究合成了新试剂2,3,7-三羟基-9-间羟基苯基荧光酮(简称m-HPF)。测定了试剂各级酸离解常数。研究了试剂的化学发光性能和试剂与金属离子的显色行为。结果表明,只有Co^2^+离子对m-HPF-H~2O~2体系有较强的催化发光作用;在表面活性剂存在下,试剂与许多离子都呈灵敏的显色反应。用Huckel分子轨道法(HMO)计算了中性分子及各离子构式的π电子分布,对离解常数进行了归属。