聚酰胺分离富集催化光度法测定痕量金

1 引 言聚酰胺是一种选择性很高的富集剂，在选择一定吸附条件下，普通金属离子不被吸附，只吸附金、银、钯、铱等贵金属离子。该法具有操作简便、吸附容量大，吸附速度快，容易洗脱，可重复使用等优点。在催化动力学光度分析中偶氮氯瞵Ⅲ作为被氧化的褪色剂应用的很多，但用于测定金未见报道。本文研究了痕量Ａｕ（Ⅲ）在稀硫酸的介质中催化溴酸钾氧化偶氮氯膦Ⅲ腿色的新指示反应及其动力学条件，建立了一种测定痕量金的新方法。方法的检出限为１．１４ × １０～（－１１）ｇ／ｍｌ，线性范围为 ０－４０ ｐｇｌＬ，该法可用于样品中痕量…     

聚酰胺富集吸光光度法测定金

ＰＶＣ－聚己内酰胺作为金的富集利，从稀盐酸或王水介中富集微量金，具有吸附速度快，容易洗脱，吸收容量大等优点，在选择的色层条件下，除贵金属和铊外，普通离子不被吸附，可广泛用于分离富集各类矿物中微量金。     

聚酰胺分离富集催化动力学光度法测定痕量金

研究了在稀硫酸介质中 ,痕量金催化溴酸钾氧化偶氮氯膦 褪色的指示反应及其动力学条件 ,据此建立了测定痕量金 ( )的新方法。方法的检出限为 1 .1 2×1 0 - 11g/m L,测定范围为 0～ 1 .0 μg/1 0 m L。采用聚酰胺在盐酸或王水介质中分离富集矿样中的金后 ,用拟定的方法测定获得满意结果     

聚酰胺和负载聚酰胺树脂富集分离环境水中无机汞

提出以聚酰胺、负载双硫腙聚酰胺、负载α-巯基苯并噻唑聚酰胺树脂为吸附剂,在静态和动态条件下,对环境水中无机汞的选择性吸附分离方法.实验表明,此3种树脂在0.1～2.5mol/L HCI介质中,对无机汞吸附性能很好,饱和吸附容量分别为:聚酰胺树脂12.28mg/g;负载双硫腙聚酰胺树脂14.48mg/g;负载α-巯基苯并噻唑聚酰胺树脂17.17mg/g.吸附到各树脂中的汞可用1%～5%硫脲溶液解脱,以冷原子吸收法测定,得到较满意的结果.     

聚酰胺富集分离-光度法测定环境样品中痕量铊

提出以聚酰胺树脂为吸附剂,在ＨＣｌ介质中,记和动态操作条件下,对环境样品中一铊的选择性吸附分离方法。树对铊（Ⅲ）有很强的吸附能力,饱和吸附容量为８．８６ｍｇ／ｇ（ｐＨ５的ＨＣｌ介质中）和０．９８ｍｇ／ｇ（１．０ｍｏｌ／Ｌ的ＨＣｌ介质中）。     

聚酰胺富集吸光光度法测定银

聚乙内酰胺作为Ａｇ的富集剂，从稀ＨＮＯ３溶液中富集Ａｇ具有吸附速度快，解脱容易，吸附容量大且可重复使用等优点。在选择条件下，最大吸附容量达５０ｍＬ／ｍｉｎ，并作１８种元素干扰实验确定允许量。     

泡沫塑料动态快速分离富集金方法的研究

本文系统研究了泡沫塑料动态快速分离富集金的方法。对泡沫塑料柱的处理方法,再生及主要共存离子干扰的消除等均做了较详细的研究。提出了一种简便,不控速的金分离富集的方法。该法用于分析0.051～3.59g/t四种不同含量的金标样,结果与推荐值吻合,5次分析结果,相对标准偏差<5％,同时,可用泡沫塑料柱当天连续使用分析拿标样,回收率为93％—109％。     

液膜分离富集金与测定微量金

提出采用乳状液膜体系分离、富集金。该体系包括协同流动载体（TBP和PMBP），表面活性剂（SPAN80），膜的增强剂（液体石蜡），膜溶剂（煤油）和内相（1％质量分数的NaOH水溶液）。实验结果表明，金的迁移率达90．5％以上。此条件下，许多共存金属高于如∑RE3+、Ag2+、Pd2+、Pt4+、Rh3+、Cu2+、Fe3+、Al3+、Pb2+、Zn2+、Mo6+、W6+、Mn2+、Sn4+、Te4+、Se4+、Ca2+和Mg2+等不被迁移，只有金能与这些金属离子得到满意的分离。该法已应用于测定提金溶液和氰化物没出贵金属溶液中的微量金，相对标准偏差为1．3％－3．9％。     

Polyamide-Coated Open- Tubular Micro-Capillary Column for Liquid Chromatography

Abstract

An open-tubular micro capillary column was prepared by coating the inner wall of a pyrex tube (50 μm i.d.) with polyamide. Chromatographic behaviors of trace amounts of various phenolic compounds, benzoic acid derivatives and aromatic amino and nitro compounds, were examined on this column.     

大口径毛细管柱气相色谱法分析三氯杀螨醇

A method of quantitative analysis for dicofol by a wide bore capillary column has been studied. The gaschromatographic conditions were as follows.Column:fused silica, HP-1(cross-linked methyl silicone)5m ×0.53mm × 2.65μm film;column temperature : 200℃;temperature of injector and detector: 250℃ and carriergas:H_2 25mL/min. Dioctyl phthalate was used as the internal standard.10% of dicofol would be decomposedquantitatively to dichlorobenzophenone.     

手性金纳米团簇:一种新型近红外荧光探针

近红外荧光成像具有低背景荧光干扰、强组织穿透力和对生物机体无光损伤等优点, 因此发展具有良好生物相容性、量子产率高、化学及光稳定性好的水溶性长波段近红外荧光探针成为目前的研究热点. 与有机近红外荧光染料相比, 无机纳米近红外荧光探针因其具有较高的摩尔消光吸光系数和荧光量子产率、抗光漂白能力强、发射光谱集中且可调等特点而备受重视. 采用N-异丁酰基-L(D)-半胱氨酸(N-isobutyryl-L(D)-cysteine, L(D)-NIBC)手性对映异构体作为还原剂和稳定剂一步法直接制备得到两种平均粒径小于2 nm的水溶性手性金纳米团簇(L-NIBC-AuNCs和D-NIBC-AuNCs). CD光谱显示二者在230~360 nm波段的圆二色性完美对称, 荧光光谱显示二者均在900~1000 nm的近红外波段具有较强的荧光发射峰, 且二者的荧光量子产率分别达到6.9% (L-NIBC-AuNCs)和8.2% (D-NIBC-AuNCs), 细胞毒性实验表明这两种手性金纳米团簇均无细胞毒性. 上述结果表明两种手性金纳米团簇不仅符合成为近红外荧光探针的基本要求, 而且还具有不对称光学活性和潜在的手性识别能力等独特性质. 手性金纳米团簇具有成为一类全新的近红外荧光探针的潜力, 为将来实现对特定分子通过手性识别来进行体内近红外荧光示踪和成像提供了全新的思路.     

A New Colorimetric Reagent for Carbon Monoxide

Abstract

A new colorimetric reagent for carbon monoxide is described. The reaction sequence apparently involves reduction by carbon monoxide of [PdCl₄]^2-, which then reduces [Fe^III EDTA]^? to [Fe^IIEDTA]^2-. The latter undergoes ligand exchange with 2,2′-dipyridyl or 1,10-phenanthroline to form the more stable colored [FeL₃]²⁺, which is measured spectrophotometrically. Sodium molybdate enhances the overall reaction. The color intensity produced is non-linear but reproducible. The method is unique in that a soluble colored compound is produced rather than a metal sol.     

Multivariate data analysis of UV spectra in monitoring elution and determining endpoint of chromatography using polyamide column

Chromatography using polyamide column is one of the most critical purification operations that affect the safety and efficacy of traditional Chinese medicine (TCM) products. To ensure successful operation and reduce time and solvent consumption, UV spectroscopy combined with multivariate data analysis as an online analytical tool was developed for monitoring the polyamide column chromatography of the TCM Danshen. The process trajectories were established by principal component analysis of the UV spectra and used to determine the endpoint of the washing stage and investigate the impacts of the process conditions. The online analysis method developed determined the concentration of salvianolic acid B (an important compound in Danshen) in the effluent rapidly and precisely with a coefficient of determination of 0.9963 and helped to collect salvianolic acid B quantitatively for determining the endpoint of elution. The methodology proposed is an effective approach applicable in guiding successful operations in the chromatographic separation.     

粮食中百草枯残留的金标免疫层析检测方法研究

采用柠檬酸三钠还原法制备胶体金,研究胶体金与抗体蛋白的作用过程,确定稳定标记1.0 mL胶体金需8.10μg抗体蛋白,标记体系的最佳pH值为8.5。以金标抗体为分析探针,PQ-h-OVA为竞争抗原,羊抗兔IgG为控制抗体,构建直接竞争胶体金标免疫层析检测体系(GICA)。确定膜上包被抗原的质量浓度为0.50 g/L,点样量为1.0μL/条;金标点样量:5.0μL/条;羊抗兔二抗的最佳包被质量浓度为0.11 g/L,点样量为1.0μL/条。金标试纸条的目测检出限为10μg/L,检测时间约5 min,交叉反应率小于0.10%。方法的重复性和稳定性较好,该试纸条在室温下至少可保存5个月。     

Mechanism of Gold Activation in Supported Gold Catalysts for CO Oxidation

Based on the structure of characterization of Au/Fe₂O₃ catalysts, the mechanism of gold activation in supported gold catalysts was proposed as follow:

A New Porphyrin for the Preparation of Functionalized Water-Soluble Gold Nanoparticles with Low Intrinsic Toxicity

A potential new photosensitizer based on a dissymmetric porphyrin derivative bearing a thiol group was synthesized. 5-[4-(11-Mercaptoundecyloxy)-phenyl-10,15,20-triphenylporphyrin (PR-SH) was used to functionalize gold nanoparticles in order to obtain a potential drug delivery system. Water-soluble multifunctional gold nanoparticles GNP-PR/PEG were prepared using the Brust–Schiffrin methodology, by immobilization of both a thiolated polyethylene glycol (PEG) and the porphyrin thiol compound (PR-SH). The nanoparticles were fully characterized by transmission electron microscopy and ¹H nuclear magnetic resonance spectroscopy, UV/Vis absorption spectroscopy, and X-ray photoelectron spectroscopy. Furthermore, the ability of GNP-PR/PEGs to induce singlet oxygen production was analyzed to demonstrate the activity of the photosensitizer. Cytotoxicity experiments showed the nanoparticles are nontoxic. Finally, cellular uptake experiments demonstrated that the functionalized gold nanoparticles are internalized. Therefore, this colloid can be considered to be a novel nanosystem that could potentially be suitable as an intracellular drug delivery system of photosensitizers for photodynamic therapy.     

新型荧光试剂柱前衍生化高效液相色谱荧光检测法测定醇类化合物

采用新型的紫外、荧光衍生试剂咔唑－9－乙基氯甲酸酯，对15种脂肪醇柱前衍生的反应条件，包括反应温度、催化剂的选择、衍生化时间等，进行了考察。结果表明：催化剂选用吡啶，反应温度80℃，时间15min，衍生化具有最大且恒定的检测响应。利用高效液相色谱对衍生产物进行分析，同时对衍生物的分离进行了优化选择，达到了较好的基线分离。检测限为13.3-93.5nmol/L。