5－Br－TAR的合成及其在反相HPLC分离测定Co（Ⅱ）、Cr（Ⅵ）、Rh（Ⅲ）中的应用

以合成的新试剂５－Ｂｒ－ＴＡＲ为往前衍生试剂，首次用阴离子表面活性剂Ｓ，Ｄ．Ｓ．为对离子试剂。以含１×１０（－２）ｍｏｌ·Ｌ（－１）的ｐＨ５．８的乙酸－乙酸钠缓冲溶液和３．５×１０（－４）ｍｏｌ·Ｌ（－１）的Ｓ．Ｄ．Ｓ．的甲醇－水（６８：３２，Ｖ／Ｖ）为流动相，在Ｃ（１８）柱上，１５ｍｉｎ内分离测定了Ｃｏ（Ⅱ）、Ｒｈ（Ⅲ）、Ｃｒ（Ⅵ）的５－Ｂｒ－ＴＡＲ配合物。当ＳＮＲ＝２时，检出限分别为０．４９、０．３２、０．４４ｐｐｂ。用于废水及电镀液中Ｃｏ（Ⅱ）、Ｃｒ（Ⅵ）的测定，效果较好。     

新荧光试剂5－（4＇－硝基－2＇－羧基苯基偶氮）－2－硫代－4－噻唑啉酮的合成及其应用研究

报道了５－（４＇－硝基－２＇－羧基苯基偶氮）－２－硫代－４－噻唑啉酮（４ＮＲＡＣＰ）的合成。经柱层析提纯，用元素分析、ＩＲ、１ＨＮＭＲ和ＭＳ确证了其结构，研究了荧光性质，发现该试剂在溴代十六烷吡啶存在下，在无水乙醇溶液中与Ｅｕ（Ⅲ）形成稳定的荧光螯合物，λｅｘ／λｅｍ＝２９０ｎｍ／３４０ｎｍ，其线性范围为１．０×１０－８～１．０×１０－６ｍｏｌ·Ｌ－１，检测限为１．５×１０－１０ｍｏｌ·Ｌ－１。测定了人工合成样品中的铕，结果满意。     

离心—光度法测定银

研究了三元配合物离心－光度测定银的新方法,在Ａｇ（Ｉ）－邻菲罗啉－溴邻苯三酚红的乙醇有色型体溶液中,于λｍａｘ＝６０６ｎｍ处测定表观摩尔吸光系数ε为４．０＊１０＾４Ｌ．ｍｏｌ＾－１．ｃｍ＾－１。     

Rh（Ⅲ）－TAC－CTMAB体系分光光度法测定Rh的研究

研究了在阳离子表面活性剂十六烷基三甲基溴化铵（ＣＴＭＡＢ）存在下，用２－（２一噻唑偶氮）－对甲酚（ＴＡＣ），在ｐＨ５．０的ＨＡｃ－ＮａＡｃ缓冲液中分光光度法测定Ｒｈ。Ｒｈ（Ⅲ）与ＴＡＣ的络合比为１：１，表观摩尔吸光系数为ε６８０ｎｍ＝１．２５×１０４Ｌ·ｍｏｌ－１·ｃｍ－１，在１．２～８μｇ／１０ｍＬ范围内符合比尔定律。方法的特征灵敏度为０．０８５μｇ／ｍＬ（１％吸收）。试验了贵金属及常见金属的干扰情况，并研究了干扰消除的方法，ＥＤＴＡ的加入可以消除一定量的Ｃｕ、Ｃｏ、Ｎｉ、Ｚｎ的干扰。对催化剂试样的分析结果令人满意，变异系数均小于３％。     

黄瓜瓜蒂组织液化学传感器研究

研制了以四（十二烷基）铵（ＴＤＡＣ）－十六烷基苄基二甲基铵（ＣＢＤＭＡＣ）－黄瓜瓜蒂组织液－丙戊酸钠为电活性物,以石墨粉为内导材料的ＰＶＣ膜电位型丙戊酸钠化学传感器。此传感器选择性、稳定性、重现性都较好。其线性范围为３．０×１０－６～１．０×１０－２ｍｏｌ·ｌ－１,检测下限为１．０×１０－６ｍｏｌ·ｌ－１,斜率为５９ｍＶ／ｐＣ（２５℃,ｐＨ＝９～１１）。     

分光光度法测定工业己内酰胺中铁

在ｐ Ｈ＝ ７ 的 Ｎ Ｈ４ Ａｃ 缓冲介质中， Ｃ Ｔ Ｍ Ａ Ｂ 微乳液存在下， Ｆｅ（ Ⅲ） 和铬天青 Ｓ 生成蓝色络合物，λｍａｘ＝ ６５５ｎｍ ，ε＝ １ ．４０ ×１０５ Ｌ·ｍｏ Ｌ－ １·ｃｍ － １ ，铁含量在０ ～６μｇ／２５ｍ Ｌ 内符合比尔定律，方法用于工业己内酰胺中铁的测定，结果满意。     

7─（4─磺苯基偶氮）─8─羟基喹啉用作钴的新光度试剂及其用于VB_（12）的间接分光光度测定

合成了题述试剂ＳＰＡＨＱ，可用其作钴显色剂。生成的红棕色１：４（Ｃｏ：ＳＰＡＨＱ）螯合物λｍａｘ＝４８０ｎｍ，ε４８０＝８．１×１０４Ｌ·ｍｏｌ－１·ｃｍ－１，Δλ＝９０ｎｍ。０～１．２μｇ／ｍＬＣｏ２＋遵守比尔定律。１～１０ｍｇ的７种离子和０．０３５～０．９４ｍｇ的１８种离子不干扰。用于间接分光光度测定ＶＢ１２，结果与亚硝基Ｒ盐法一致。本法既灵敏、选择性也好。     

CPARH的合成及Ag（Ⅰ）－CPARH络合物的光度性质研究

合成了５－（２－（４－氯苯酚）偶氮）－罗丹宁。在ｐＨ６．９５的ＮＨ４Ａｃ缓冲溶液中，当有０．１８％的ＳＬＳ存在时，Ａｇ（Ⅰ）与ＣＰＡＲＨ形成１：１络合物，λｍａｘ为４８０ｎｍ，ε为１．０×１０５Ｌ·ｍｏｌ－１·ｃｍ－１，Ａｇ（Ⅰ）含量在０．０１１～５．４０μｇ／ｍＬ范围内服从Ｂｅｅｒ定律。所提出的方法用于精铜矿中微量银的测定，相对误差在５．０％以内。     

新显色剂7-(苯并噻唑-2-偶氮)-8-羟基喹啉-5-磺酸的分析性能及其与锌显色反应的研究

报道了新显色剂７－（苯并噻唑－２－偶氮）－８－羟基喹啉－５－磺酸（简称ＢＴＨＱＳＡ）的离解常数的测定，同时研究了该显色剂对锌离子光度分析的条件，摩尔吸光系数ε＝５．１×１０４Ｌ·ｍｏｌ－１·ｃｍ－１，锌离子浓度在０～６．５μｇ／２５ｍＬ符合比尔定律，并对人发中的微量锌进行测定。     

新显色剂4—（2—吡啶偶氮）—邻苯二酚吸光光度法测定微量Hg（Ⅱ）

研究了新显色剂４－（２－吡啶偶氮）－邻苯二酚（ＰＡＣＰ）与Ｈｇ（Ⅱ）的显色反应。在阳离子表面活性剂溴化十六烷基三甲胺（ＣＴＭＡＢ）及ｐＨ＝９．５ＮＨ３－ＮＨ４Ｃｌ缓蚀溶液中,试剂与Ｈｇ（Ⅱ）反应生成稳定的红色配合物,其最大吸收波长为５０３ｎｍ,表观摩尔吸光系数为３．０×１０＾５Ｌ·ｍｉｌ＾－１·ｃｍ＾－１,汞含量在０～３．０×１０＾－６ｍｌｏ·Ｌ＾－１范围内服从比耳定律,该方法应用于合成样和废水中     

Analysis of forming process of nitrogen-doped carbon catalyst derived from Fe 1,10-phenanthroline compound and its oxygen reduction reaction activity

The pyrolysis behavior of iron 1,10-phenanthroline compound, the change of crystalline structure of iron in the iron 1,10-phenanthroline compound, and nitrogen chemical state of nitrogen doped carbon catalyst derived from iron 1,10-phenanthroline compound were investigated to clarify the process of improvement of oxygen reduction reaction (ORR) activity on nitrogen-doped carbon catalyst by TGA, EGA-MS, HT-XRD, XRD, and XPS technique. The ORR activity drastically improved at a synthesis temperature of 700 °C, and was the highest at a synthesis temperature of 800 °C. But the ORR activity significantly dropped at a synthesis temperature of 900 °C. This low ORR activity of NC-900 is probably due to the increase of quaternary nitrogen ratio with progression of excessive carbonization, and the quaternary nitrogen to pyridine-like nitrogen ratio might be an important factor for improvement of the ORR activity.     

3,4,5-三甲氧基苯甲醛缩乙醇胺席夫碱合成,表征与抑菌活性研究

合成了3,4,5-三甲氧基苯甲醛缩乙醇胺席夫碱,并对其进行了结构表征,初步确认了其组成,抑菌实验表明该席夫碱对枯草杆菌、大肠杆菌、金黄色葡萄球菌、革兰氏阴性细菌(发荧光Q67)均有较好的抑制作用。     

间接分光光度法测定盐酸羟胺

拟定了在铁（Ⅲ）－邻菲罗啉络合物存在下盐酸羟胺的间接分光光度测定方法,回收试验表明拟定方法准确可靠,方便快捷。同时测定了盐酸羟胺与铁（Ⅲ）－邻菲罗啉络合物的反应比     

UV/HA与铁盐体系对染料的脱色研究

水溶性染料活性艳红（Ｘ－３Ｂ）在铁盐与腐植酸共存下,光解脱色效果明显,结果表明在ＰＨ＝３,１．０＊１０＾－５ｍｏｌ／ＬＦｅ（Ⅲ）与０．５ｇ／Ｌ腐植酸的条件下,２０ｍｇ／Ｌ活性艳红溶液的脱色率为７１．４％。染料溶的ＰＨ值,Ｆｅ（Ⅲ）,腐植酸的浓度以及当杰溶液的初始浓度均对染料的脱色有影响。     

Preparation and properties of Fe(II)‐ion‐sensitive colour‐changing fabric

Textile fabrics were dyed with complexometric indicators (ionochromic dyes) to develop Fe(II) ionochromic fabric. Three kinds of ionochromic dye were used to dye silk fabric, and they were evaluated for colour changes triggered by Fe(II) solution. The K/S values and photos of the fabrics were then recorded. It was found that 1,10‐phenanthroline was the most suitable ionochromic dye in these dyes. Colour change from white to red could be clearly seen when 1,10‐phenanthroline‐dyed silk fabric was triggered by Fe(II) solution, but it showed no colour change when triggered by Cu(II), Mg(II), or Ca(II) solution. Moreover, 1,10‐phenanthroline‐dyed nylon, polyester, and cotton fabrics showed no obvious colour changes after triggering by Fe(II) solution. Ion concentration, pH value, and reaction time could affect the colour changes. When triggered by 8 mg l^?1 of Fe(II) solution at neutral pH for about 15 min, the ionochromic fabric showed a clear colour change. In addition, three coloured fabrics in green, blue, and yellow were also dyed with 1,10‐phenanthroline. It was found that they could also show clear colour changes when triggered by Fe(II) solution. These ionochromic fabrics may find broad application in many fields, such as Fe(II) detection, magic toys, anticounterfeiting materials, and bionic silk flowers.     

片状电子级碳酸钡的制备与烧结性能

以廉价的氯化钡和碳酸铵为原料制备碳酸钡,研究了工艺条件对产物晶体形态及粒径的影响,制得了具有良好分散性能的片状电子级碳酸钡。与ＴｉＯ２混合后的煅烧产物ＢａＴｉＯ３粒度小,结晶性好。烧结成的电子陶瓷具有优良的电学性能。     

Colorimetric sensor based on polymeric thin film for arsenic quantitation using colour response calibration

A simple, low-cost and portable sensor for colorimetric determination of As(III) was developed. The sensing is carried out using a microcentrifuge tube as a mini-reactor, where an Fe(III)-1,10-phenanthroline doped polyvinyl alcohol thin film is cast on the underside of the cap. Once Fe(III)-1,10-phenanthroline is reduced by arsine gas generated in situ from As(III), yielding the Fe(II)-1,10-phenanthroline complex, the red coloured product can be detected using colour analysis software. The As(III) content is then determined based upon the colour intensity of Fe(II)-1,10-phenanthroline on the film. Experimental conditions were optimised, and parameters affecting the complex formation and arsenic speciation were investigated. The method developed proved to be a selective colorimetric sensor for As(III). More significantly, the device could be directly used to detect As(III) in the field without any sample preparation requirements. The recovery for industrial wastewater and groundwater was found to be 97.5%-104.0%. Hence, the thin film-based test kit is easy to operate, portable and practical for the measurement of As(III) in the field.     

动力学分光光度法测定食品中的痕量铁

介绍了一种动力学分光光度测定痕量铁的方法。在ｐＨ＝４．７０的ＨＡｃＮａＡｃ介质中,Ｆｅ（Ⅲ）对Ｈ２Ｏ２氧化番红花Ｔ的反应具有强烈的催化作用,使溶液颜色褪去。该溶液最大吸收波长为５２０ｎｍ,铁含量在３．０８×１０６２．８０×１０５ｇ／Ｌ范围内遵从比尔定律,表观摩尔吸光系数为５．６×１０５Ｌ·ｍｏｌ１·ｃｍ１,回归方程为：ΔＡ＝５．６×１０５ＣＦｅ（Ⅲ）＋０．０２（Ｃ的单位为ｍｏｌ·Ｌ１）,相关系数γ＝０．９９９９,检出限为３．１６×１０６ｇ／Ｌ,同时也研究了多种干扰离子对测定的影响,该方法应用于测定食品如大米、面粉中的痕量铁取得了满意的结果     

聚乙二醇—硫酸铵—邻二氮菲体系萃取光度法测定铁的研究

建立了在聚乙二醇—硫酸铵—邻二氮菲体系中非有机溶剂萃取光度法测定铁的新方法 ,方法基于在 p H=5.8的缓冲溶液中 ,低价铁与邻二氮菲形成稳定的 1∶ 3的配合物 ,被萃取到高聚物相 ,其配合物的最大吸收波长位于 50 8nm、摩尔吸光系数ε=1 .1× 1 0 4 ( mol· cm) -1。在铁含量为 0～ 50μg范围内服从比尔定律 ,此法已用于生物样品中微量铁的测定 ,结果满意     

Isolation of a trimer of α-tocopherol from mammalian liver

Evidence is presented for the formation in mammalian liver of a trimeric metabolite of α-tocopherol. This compound has been shown to be identical to a trimer produced by oxidation of α-tocopherol with alkaline K₃Fe(CN)₆. In addition, confirmation was obtained for the occurrence in vivo of a dimeric metabolite reported previously. These compounds, together with tocopheryl-p-quinone, are postulated to arise from reactions with lipid-free radicals or peroxides in the course of the antioxidant action of vitamin E.