两次金汞齐—冷原子吸收光谱法测定雨水中不同形态汞

本文建立了两次金汞齐冷原子吸收光谱法测定雨水样品中总汞及活性汞、次活性汞和惰性汞的方法,该方法的最低检出限为０．５ｎｇ．ｌ＾－１,回收率为９６－１０５％,精密度ＲＳＤ≤５．３％,该方法还可用于其它天然水体中汞的形态测定。     

用化学发光法测定雨水中的氨

本文研究了用ＴＣＰＯ－Ｈ２Ｏ２发光体系对氨进行测定。结果表明，当ｐＨ＝１０．３，ＯＰＡ浓度为１０ｍｍｏｌ．ｌ＾－１，氨浓度在０－６ｍｇ．ｌ＾－１时，其浓度和发光强度有良好的线性关系（相关系数为０．９９８），本法的最低检出限为２ｎｇ．ｌ＾－１。可用于实际雨水样品的测定，测定结果还表明：本法具有灵敏度高，精度高，线性范围宽干扰少等优点，适用于大批量分析及连续自动监测分析。     

改性绿茶对汞的吸附研究——汞的形态分析

试验了用改性绿茶分离，冷原子吸收光谱法测定无机汞，烷基汞和苯基汞的条件。在ｐＨ５的溶液中吸附无机汞，与有机汞分离；在ｐＨ１的溶液中吸附有机汞，然后分别以１．５，３．０和６．０ｍｏｌ·１＾－１盐酸解吸无机汞，烷基汞和苯基汞，用冷原子吸收光谱法测定汞，探讨了吸附机理，分析了牡蛎和水样中汞的形态。     

二甲基硫醚的真空紫外光电子谱

本文测定了二甲基硫醚（ＤＭＳ）的真空紫外光电子能谱（ＵＰＳ），实验测得的ＤＭＳ的各Ｉｖ（ｃＶ）值与Ｋｉｍｕｒａ的结果一致。８．７９，１１．２９ｅＶ峰指认为硫原子孤对电子ｎｇ，ｎｓ的电子电离，１２．６２ｅＶ峰相应于σｃｓ价电子电离，１４．０３－１５．４２ｅＶ的四个峰相应于πＣＨ３－，πＣＨ３＋电子电离，紫外光辐照影响ＤＭＳ的ＵＰＳ，显示在πＣＨ３有变化。微波放电时ＤＭＳ的ＵＰＳ有明显的影响，有许多新     

电感耦合等离子体—质谱法测定成人脏器样品中痕量稀土元素的研究

本文采用ＩＣＰ－ＭＳ法对成人脏器样品中痕量稀土元素进行了研究，选择了测定的最佳仪器参数，检查了测定中的各种干扰和影响；用铼（Ｒｅ）为内标元素补偿基体抑制效应和灵敏度的漂移。方法对稀土元素各分量的检出限为０．００５－０．０２６ｎｇ．ｍ１＾－１，标准回收率为９２．９－１１１．３％，精密度为０．９６－３．０７％。在严格分析质量控制的基础上用混合酸消解样品，不须分离富集，直接对成人的心、脾、肝、肾、肺肉中     

流动注射在线萃取—火焰原子吸收光谱法测定人发中微量镉和铅

本文建立了一个流动注射在线萃取－火焰原子吸收测定人发中微量镉和铅的方法，对含Ｃｄ和Ｐｂ分别为０．０２μｇ／ｍｌ和０．２０μｇ／ｍｌ的溶液，其相对标准偏差分别为３．４％和３．８％（ｎ＝９），Ｃｄ和Ｐｂ的灵敏度分别提高２１倍和２３倍，分析速度达３６次／ｈ，Ｃｄ和Ｐｂ的回收率分别在８７．３％－９７．０％和９１．９％－１０７．３％之间，文中还详细研究了各种实验参数的选择，测定人发样的结果与文献值相符。     

土壤中残留苯磺隆的高效液相色谱分析

本文报道了一种固相萃取净化，高效液相色谱测定土壤中苯磺隆的残留分析方法，不同土壤的添加回收率平均为８３．３％，８６．３％，７７．２％，线性范围２．５５－５１０ｎｇ，利用本法分析苯磺隆，精确、简便、快速。     

土壤中绿磺隆残留量生物测定方法

用生物测定方法测定了土壤中绿磺隆残留量，建立了绿磺隆浓度（Ｙ）与玉米根长（Ｘ）之间的相关模式：Ｙ＝３０．５６２－３６．３８ＩｎＸ＋１４．８２８（ＩｎＸ）￣２＋２．０４３（ＩｎＸ）￣３．此模式适用于土壤中０．１～４．０μｇ／ｋｇ浓度范围的绿磺隆残留量测定，最低检出量为０．１μｇ／ｋｇ。     

流动注射荧光分析法用于土壤及水系沉积物中铈（Ⅲ）含量的测定

研究表明Ｃｅ＾３＋在ｐＨ〈６．２ＫＣｌ介质中以２５４．０ｎｍ紫外光激发时，在３５２．０ｎｍ处发出具有恒定强度的荧光。因而可选择ｐＨ５－６作为测定酸度条件，利用Ａｌ２（ＳＯ４）３消除Ｆｅ＾３＋等离子的干扰，建立起Ｃｅ＾３＋的流动注射荧光分析法。方法的线性范围是２．０×１０＾－７—２．０×１０＾－６ｍｏｌ／ｌ，一元回归方程△Ｆ＝６６３６００Ｃ－０．０４１（ｎ＝１０，ｒ＝０．９９９７），检测限６．０×１     

几种汞的分析方法简介

原子吸收分光光度法 目前的文献中有各种有关汞的分析方法,其中尤以无火焰原子吸收法为多。Hatch和Off用氯化亚锡将汞离子还原为元素汞,而后将其以空气载入原子吸收池来测定溶液中汞是具有代表性的一种方法。Vaughn和Mccarthy将土壤、矿石、气体的含汞气流通过500℃以上的金丝捕样网而测定无机、有机汞。     

Distribution of mercury in the sediments of some freshwater bodies in Ethiopia

Sediment samples were collected from Tinishu Akaki River (TAR), Lake Awassa, and Lake Ziway, Ethiopia for determination of mercury. The air-dried samples were analyzed for mercury with a differential atomic absorption spectrometer after thermal evaporation of bound mercury converting it to its atomic form. Certified reference materials (CRMs) of sediments and soils were used to validate the method. The recovery of mercury from CRMs and sediments was in the range of 95–100%. The limit of detection for the determination of mercury was 50?ng?kg^?1. The concentration of total mercury in the sediments varied from 3.9 to 110?µg?kg^?1 for TAR, 14 to 67?µg?kg^?1 for Lake Awassa, and 17 to 110?µg?kg^?1 for Lake Ziway. It was found that the total mercury concentrations in all samples were below the United States Environmental Protection Agency guideline of 200?µg?kg^?1.     

Reagenzienfreie Bestimmung von Quecksilberspuren in Wasserproben

A comprehensive ecological monitoring of hazardous substances is indispensable to preserve our health and environment. Therefore, fast and inexpensive techniques for routine analysis of pollutants are essential. However, in the measuring procedure itself often toxic reagents are used producing hazardous waste. Omitting environmentally hazardous substances in the analysis procedure is an important contribution to a more sustainable and green analytical chemistry. A reagent-free method for ultra-trace (pg to ng?L^-1) mercury determination in water samples was developed and validated. An active nanogold collector integrated in a fully automated flow injection system is the core of this new method. All mercury species dissolved in the water sample are adsorbed and preconcentrated on the nano-structured gold surface of the collector. After rinsing and drying of the collector, the enriched mercury is thermally desorbed and finally measured by atomic fluorescence spectrometry. This method was optimized and validated for the determination of mercury in natural waters. The influence of various water constituents was investigated and only high contents of dissolved organic carbon (DOC) showed interferences of mercury preconcentration due to the strong complexation of mercury by DOC. This restriction can be solved by UV-irradiation, i.?e. reagent-free digestion of DOC rich samples prior to the preconcentration procedure. Mercury concentration of several natural river and sea waters and water from the discharge of a waste water treatment plant were determined with this new analytical method. Accuracy and precision of the method were demonstrated by several recovery experiments in natural water samples (recoveries: 96–102?%) and by analysis of the certified reference material BCR-579 (Mercury in Coastal Sea Water; recovery: 101?±?1?%). With a detection limit of only 80?pg?Hg?L^–1 the proposed method is highly sensitive. Furthermore the method avoids potential contamination of the sample by reagent addition and is due to the reagent-free procedure environment-friendly. Hence this work is an important contribution to sustainable environmental analysis and at the same time improves accurate routine mercury trace analysis.     

Estimation of mercury speciation in soil standard reference materials with different extraction methods by ion chromatography coupled with ICP-MS

Analytical methods for the speciation of mercury, based on microwave extraction and sonication extraction, have been tested to determine the inorganic mercury and methyl mercury contents in two standard soil reference materials: SRM 2710 Montana Soil and BCR 580 estuarine sediment. Prior to applying the speciation extraction methods, the mineral compositions were analyzed via XRD analysis, with SRM 2710 shown to be composed mostly of aluminum silicate minerals, while carbonate minerals were the major constituent in BCR 580. Two extraction methods, microwave and sonication, were tested for the analysis and recovery efficiency of total mercury. The accuracy and efficiency of each extraction method was also compared. In the analysis of total mercury, the microwave extraction method, with using methanol and HCl as extractants, was better for SRM2710, while the application of the sonication extraction method was more efficient for the calcite-based BCR 580. The results showed good separation and recovery efficiencies, with values reaching 100% of those estimated. The sonication method was selected for the speciation of mercury, especially in BCR 580. An extraction solution comprising of a 1:1 mixture of methanol and HCl was used for the sonication extraction of BCR 580, with the resulting extractants analyzed by IC-HG-ICP-MS for methyl mercury and inorganic mercury. As a simple, rapid, sensitive, and accurate method, sonication extraction was found to be satisfactory.     

Mercury fractionation in the sediments of Vembanad wetland, west coast of India

Transformations among different mercury species associated with sediments can have a major effect on the metal's mobility and potential for methylation and hence bioaccumulation. In the present study, various fractions of mercury in the sediments of Vembanad wetland system analysed. Total mercury (THg) concentration in the surface sediment varied from 16.3 to 4,230?ng/g. The results of sequential extraction showed that the major portion of mercury in these sediments existed as elemental form followed by organo-chelated form. The least portion observed was the residual fraction (mercury of natural origin). Even though the percentage of mercury observed in the easily available fractions is relatively small, absolute values of these mobile Hg fractions are quite high due to the very high total mercury values. The fractionation of mercury in the sediment was controlled by the organic matter, sulphur complexes and concentration of THg. The results showed that the bioavailability of mercury is high as the amount of mercury found in the initial three fractions is high, which can also enhance the methylation potential of the Vembanad wetland sediments. The fractionation pattern of mercury also revealed the presence of anthropogenic mercury content in the Vembanad wetland sediments.     

封闭垃圾填埋场通过地表向大气释放汞的测定

利用动力学通量箱及自动测汞仪联用技术,于2004年3月中旬对贵阳市的一座封闭生活垃圾填埋场汞通过地表向大气释放的过程进行了研究。3个采样点的汞释放通量日均值分别为559.1、88.2、53.6ng·m-2·h-1,汞释放通量强度与表层基质中的汞含量密切相关,该测定值高于世界背景地区通量的1~2个数量级,说明封闭垃圾填埋场也是大气汞的潜在来源。汞释放通量呈现明显的昼夜变化规律,白天较高并在午间前后达到最大,而夜间降至最低。气相因子中光照强度与汞的释放过程相关性最高,其次分别是气温、相对湿度、地温和风速。氧化态汞的光致还原作用是可能垃圾填埋场Hg0生成的主要途径,降雨初期能促进地表汞的释放。     

北京市场常见水产品中总汞、甲基汞分布特征及食用风险

以甲苯二次萃取-直接测汞的方法对北京市场常见水产品中的甲基汞进行分析测定,并评价了食用人群的暴露风险。分析样品包括大黄鱼（Pseudosciaena crocea）、虾（Penaeus chinensis）等9种常见海产品以及武昌鱼（Megalobrama amblycephala Yih）、鳙鱼（Aristichthys nobilis）2种淡水海产品。测定结果表明：海产品中总汞和甲基汞质量分数要远高于淡水鱼中的总汞和甲基汞质量分数,总汞绝大多数是以甲基汞的形式存在,所占比例从74.7%到96.0%不等;对其中3种鱼类的鱼体甲基汞分布研究表明：肌肉中的甲基汞质量分数最高,肝脏中次之,鱼鳃中质量分数最低。根据我国水产品甲基汞标准,本研究中水产品甲基汞质量分数均低于国家标准,但根据世界卫生组织（WHO）和美国环保署EPA颁布的甲基汞摄入量参考值,食用银鳕鱼等甲基汞质量分数相对较高的水产品仍然存在一定的风险,应注意限量。     

长江口湿沉降汞的时间分布及潜在生态危害

于2008年2月-2009年1月逐月采集长江口右岸陈行采样点的大气湿沉降样品,测试样品的总汞、溶解态汞浓度。分析结果显示,不同月份湿沉降中各形态汞的浓度变化较大,其中总汞浓度变化范围在0.09-0.45μg/L,体积加权平均值为0.22μg/L,总汞沉降通量高达199.79μg/（m2.a）,远高于其它地区,该区域的大气已经受到一定程度的汞污染。总汞、颗粒态汞月沉降量与降水量呈明显的正相关关系（除6月份）,总汞浓度与降水量在汛期（6-9月份）具有良好的负相关性,大气湿沉降汞的形态受到人为活动产生的颗粒物的影响,颗粒态汞占总汞比例变化范围在14%-89%之间,平均为62%。以地表水Ⅲ类标准0.1μg/L为评价标准,长江口湿沉降汞的潜在生态危害系数高,全年湿沉降汞平均值属于强生态危害范围。     

A fast and reliable method for quantitative determination of total mercury in vegetables

A cloud-point extraction (CPE) process using the nonionic surfactant, polyethylene glycol tert octylphenyl ether (Triton X-114) was employed for determination of Hg(II) ions in aqueous solutions. The method is based on the ion-pairing reaction of Hg(II) with Pyronin B (PyrB⁺) in the presence of excess iodide at pH 6.0 and extraction of the complex formed. The chemical variables affecting CPE efficiency were studied, and the analytical characteristics of the method were obtained. The calibration curves were linear in the range of 1–40 μg L^?1 with the detection limits of 0.35 and 0.30 μg L^?1 at 556 and 521 nm. Selectivity was also tested. The coefficients of variation of the method are 2.4% and 5.2% for five replicate measurements of mercury at levels of 10 and 25 μg L^?1, respectively. The results obtained for two certified reference samples were in a good agreement with the certified values. The method was applied to the determination of total mercury in vegetable samples.     

空气整段间隔流动注射-催化动力学光度法测定天然水中痕量钒

应用空气整段间隔流动注射法与改进的钒-溴酸钾-没食子酸催化动力学反应体系相结合,建立了测定天然水体中痕量钒的催化动力学光度FIA法。通过使用一个自制的进样阀,使样品带在反应管道中的留存时间得到延长,加热允许温度得到提高。在温度80℃,反应留存时间4.75min条件下,可测定0—10ppb的钒,检出限达0.1ppb。测定2ppb钒样品时,RSD为2.7％(n=10),测定频率达90次/h,方法的平均回收率在80—109％之间。     

Distribution of mercury in the atmosphere over Idrija, Slovenia

Idrija mine, the second largest mercury mine in the world, was in use since 1490. More than 107 000 tons of Hg were produced in its five centuries of history until 1990 when production was reduced to a few hundred kilos per year. The average recovery rate of mercury has been estimated to 73%; much of the remaining 27% was dissipated into the environment. In spite of present minimal levels of production, and only a few days of smelter operation per year, a real time survey with a mercury Zeeman analyser in a car showed relatively high mercury concentrations in the air. Amounts of 300--4000 ng Hg ^m-3 have been found around both the major sources of mercury vapour, the smelter and mine ventilation shaft -- while the amounts at the Old Place, at the City Museum, and near the Nikova-Idrijca confluence are of the order of 50 ng m^-3. Polluted air will be transported from those sources to a degree which depends on the weather conditions, mainly the direction and intensity of the wind. The high mercury contents in the air are not only due to anthropogenic sources (smelter and the ventilation shaft, dumps and smelter slag used in construction), but may also partly be natural as in the Pront area, where the outcropping bedrock contains native mercury.