原子荧光光谱半自动系统对有机汞和无机汞的分析1 - Windows Live

原子荧光光谱半自动系统对有机汞和无机汞的分析1

The present work describes an improved method for the determination of total and organic mercury by decreasing analysis time (use of a dual circuit), sample size, and handling procedures and eliminating the need for a clean room condition while maintaining the detection limit below the parts per trillion (pptr) level. Total mercury was analyzed after reduction by a one-stage gold amalgamation before transfer to an atomic fluorescence spectrometer. The detection limit was 0.07 ng L-I for aqueous samples and 1 ng g1 for biological tissue. Analysis time was 5 min. Organic mercury was first derivatized using sodium tetraethylborate and then trapped onto a graphitized carbon trap before transfer to an isothermally controlled GC column coupled to a cold vapor atomic fluorescence spectrometer. The detection limit for methylmercury was 0.05 ng L-I for aqueous samples and 1.4 ng g1 for biological tissue. Samples were analyzed in 10 min. The outlined analytical protocol permits a semiautomation of both inorganic and organic mercury analyses.
目前的工作旨在描述一种检测总汞和有机汞的改进方法,该方法使用更少的分析时间(采用对偶电路),分析更少的试样量,采用更简短的分析步骤而无需一个清洁房间,却可使检测分析达到ppt级。在放入自动原子荧光光度计前,使用黄金融和而使总汞减少。检测极限分别为:含水试样0.07ng/L,生物组织1ng/L。分析时间为5分钟。有机汞首先使用四乙基硼酸钠XXX,然后由石墨碳装置捕获,并通过连接着冷原子荧光光度计的等温吸附GC柱。检测极限分别为:含水试样甲基汞0.05 ng/L,生物组织1.4ng/L。样品分析时间在10分钟内。有机汞和无机汞的分析图象均采用半自动化方式完成。

The ability to determine mercury either as total or organic mercury below the parts per trillion (pptr) (ng L-I) level has become a major need in recent years. Researchers in Sweden and North America have shown that in aquatic environments, where mercury concentrations in the water column are often below the pptr level, the concentration of mercury in fish ranges from 0.5 to 2 μg /g (mainly as methylmercury).lS2 This is the result of two important processes: methylation of inorganic mercury and its biomagnification through the food chain. To understand these environmental processes (mercury chemistry, biotransformation, bioavailability, and bioaccumulation) quantification of the different species of mercury, in the water column, sediments, and biota is, therefore, a high priority.
近年来对于总汞或有机汞低于ppt级含量的检测需求成为主流。瑞典和北美国家的研究者发现,在水生环境中水中汞的含量通常在ppt级以下,而在鱼体内浓度在0.5-2μg/g间(主要以甲基汞形式存在)。这主要由两个重要过程:无机汞的甲基化和通过食物链生物放大。需对不同物种富集汞进行量化,以更好得了解这些环境过程(汞化学性质,生物转化,生物药效率,生物体内积累)优先考虑水体、沉积物和生物体。
In recent years, many methods for metallic mercury and organic mercury determinations have been published. A comparison of selected methods is given in Table 1. For total mercury the lowest absolute detection limit (DL), 0.09 pg, (was obtained in less than 1 min by laser-excited atomic fluorescence spectrometry with electrothermal atomization.) However, because of the small size of the sample to be used (only 10 μL), the detection limit in water was only about 9 ng L-l. For organic mercury determinations, most of the techniques are based on selective reduction (addition of an oxidative reagent vs no addition), complexing with organic molecules (ammonium tetramethylendithiocarbamate, 2-mercaptobenzothiazole,
et^.) and HPLC or GC separation (see Table 1).?

近年来,发表了许多测定金属汞和有机汞的方法。表1对一些常用方法作了一下对比。对于总汞的的{jd1}探测极限为0.09pg,(利用电热离解并通过激光激发原子荧光光谱法测定)。由于使用的试样量很小(10μL)水中探测极限为9ng/L。对于有机汞探测极限来讲,大多数技术基于选择性还原(加入氧化剂比之不加),与有机分子配位(XXXXX)和HPLC或GC分离。

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