卟啉配合物-巯基棉体系分光光度法测定中药中铅、镉、铜

研究了卟啉与铅、镉、铜的反应及配合物的电子吸收光谱。结合巯基棉分离富集方法 ,将此金属卟啉配合物体系成功地应用于中药中微量铅、镉、铜的测定。方法简便 ,测定体系抗干扰的效果好 ,灵敏度高。实际样品测定的RSD在 3 3%～ 9 6 %之间。样品加标回收率在 90 %～ 1 0 3%之间。     

重金属离子对牛胰核糖核酸酶的作用机理

通过在核糖核酸酶介质中加入Ce^3 ，Cd^2 ，Pb^2 ，研究其对核糖核酸酶活性影响的作用机理。结果表明低浓度重金属离子对酶活性有激活作用，高浓度则严重抑制酶活性。荧光滴定表明在一个Rnase分子上结合一个Ce^3 、或三个Cd^2 、或三个Pb^2 ，因而导致了酶的构象改变，酶失去活性。     

缝管捕集原子吸收光谱法测定环境样品中微量Pb,Cu和Cd

研究了缝管原子捕集原子吸收光谱法测量Ｐｂ、Ｃｕ和Ｃｄ的最佳条件。结果表明，在选定的条件下，捕集１ｍｉｎ，测得Ｐｂ、Ｃｕ和Ｃｄ的特征浓度分别为１８２×１０－３、１２６×１０－３和６７×１０－５ｍｇ／Ｌ，比常规火焰原子吸收光谱法的灵敏度分别提高１１０、３９和１５０倍，用本方法测定地表水、茶叶和人发等环境样品中的微量Ｐｂ、Ｃｕ和Ｃｄ，结果满意。     

悬浮体进样-基体改进效应石墨炉原子吸收光谱法直接测定土壤中的铅和镉

建立了以悬浮体进样-基体改进效应石墨炉原子吸收法测定污灌区土壤中痕量铅和镉的新方法。以琼脂为悬浮剂、NH₄H₂PO₄作基体改进剂,研究了土壤悬浮液的稳定性和基体改进效应及干扰效应。基于原子化峰值时间的对数值与原子化温度之间的线性关系测得Cd和Pb的表观活化能,探讨了基体改进效应机理。应用标准曲线进行校准, Pb和Cd的检出限分别为9.05×10-10 g·mL-1和1.76×10-11 g·mL-1,Pb和Cd的回收率分别为91%～97%和93%～109%,相对标准偏差为4.2%～7.8%。以土壤标准品作参照, 测得值与标准值相符。     

Determination of Pb,As, Cd and trace elements in polluted soils near a lead–zinc mine using polarized X‐ray fluorescence spectrometry and the characteristics of the elemental distribution in the area

Polarization energy dispersive X‐ray fluorescence spectrometry was used in the determination of Pb, As and Cd, as well as Cr, Cu, Zn, Ni and other minor and trace elements in the soil samples taken from a polluted area by lead mine exploitation. Two difficulties have to be overcome. One is strong overlap of Pb Lα over As Kα and another is lack of suitable certified reference materials. The different excitation conditions and analytical lines were tried to reduce the impact of overlap of Pb Lα over As Kα. When KBr was used as the second target, compared with Zr, the proportion from Pb Lα was reduced about six times. Even so, however, the overlap was not reduced enough to be ignored. The inductively coupled plasma atomic emission spectrometry and mass spectrometry methods were used to analyze parts of soil samples and provide data for compensating lack of reference materials. By this method, the analytical concentration range of Pb, As and Cd were significantly extended. The analytical range of Pb, As and Cd were 1.4 µg/g~4.2%, 0.6 µg/g~9.3% and 0.5 µg/g~1500 µg/g, respectively. The high concentrations of Pb, As and Cd were found in the samples in the vicinity of the Pb‐Zn mine. The concentrations of Pb, As, Cd, Zn and Cu were higher than the Class III in the Chinese environmental quality standard for soils. The highest concentrations of Pb, As, Cd and Zn in the soil samples were 14 960, 2726, 65 and 9439 µg/g, respectively. Copyright © 2012 John Wiley & Sons, Ltd.     

转小鼠金属硫蛋白(MT)基因烟草不同器官中金属离子铅和锌的分布

转金属硫蛋白(MT)基因植物具有清除重金属污染的能力,但是金属离子在植物体内的分布研究较少。文章以多代培育纯合的转MT烟草为材料,研究了转MT基因烟草积累铅和锌以及铅和锌在不同器官的分布情况。结果表明转基因植株的老叶、茎部和根部铅和锌积累量显著高于普通烟草植株,整株的铅和锌含量分别提高了21.8%和27.2%。铅和锌在植物体内的分布也发生了变化,转基因植株老叶和根中的铅含量分别高出普通烟草同位置的30.2%和47.8%,锌在转基因植株老叶、茎和根中的含量分别高出普通烟草同位置的44.7%,29.2%和21.6%,说明铅更容易在转基因植株老叶和根中积累,而锌更容易在转基因植株的老叶和茎中积累。     

Evaluation of metal release from battery and electronic components in soil using SR‐TXRF and EDXRF

Potentially toxic elements may be leached contaminating the soil, surface, and ground water due to the improper disposal of batteries and electronic devices. The objective of this study was to evaluate metal release from batteries and electronic components deposited in specific receptacles filled with soil in which acid rain was simulated. The leachate solution and the soil were analyzed by synchrotron radiation total reflection x‐ray fluorescence and benchtop energy dispersive x‐ray fluorescence, respectively. Results indicate that batteries released K, Mn, Fe, Cu, Zn, and Pb and electronic component released Ti, Mn, Fe, Cu, Zn, and Pb. For batteries' leachate test samples, higher amounts of Fe, Cu, Mn, Zn, and Pb have been released compared with electronic component ones under same the experimental conditions. The Fe, Cu, and Pb concentrations in battery leachate test samples were above their National Environment Council maximum permitted values (MPV) and in the electronic waste leachate ones, only the Pb concentrations was above MPV. For soil sample containing batteries K, Mn and Zn presented higher concentrations, mainly at the 10‐cm topsoil, ranging from 0.16 to 0.50, 0.27 to 8.67, and 0.03 to 1.26, in % (% w/w), respectively. The Zn–C battery soil samples present similar behavior to the alkaline ones. The impact due to the Pb release was higher in the soil test samples with electronic components, in which their concentrations ranged from 51 to 394 mg/kg, above its MPV up to 28‐cm soil layer. The X‐ray fluorescence techniques employed were suitable for water and soil environmental evaluation.     

SR-XRF analysis and assessment in urban ecology studies: The case of Novosibirsk

This paper considers the elemental composition of aerosols which have accumulated in the snow in winter and that of the top soil layer (0–5 cm), birch (Betula pendula Roth.) leaves collected at the end of the vegetative season, and soils in the vicinity of Novosibirsk. The analysis is carried out using the X-ray fluorescence elemental analysis with synchrotron radiation (SR-XRF) method, which helps reveal the existing local aerosol pollution from industrial sources. The main geochemical indicators of aerosol pollution of the Novosibirsk tin smelter (Novosibirskii Olovokombinat) are As, Sn, Tl, Cd, and Pb; those of three Novosibirsk heat power stations TETs-2, -3, and -5 are V, Mn, I, and Ga. It is found that the accumulation of the majority of technogenic elements in the tissues of higher plants depends on the intensity of the pollution, except for the biophilic Cu, Zn, and Mn, the content of which is more regulated by the physiobiological mechanisms of plants. For example, birch leaves are found to have a lower Mn content in the areas of high technogenic pollution, whereas, in ecologically clean areas, the Mn content in plant tissues is observed to increase. Thus, in Siberia, the snow cover and vegetation are the seasonal depositing components of the urban environment that adequately reflect the existing technogenic aerosol pollution. The elemental SR-XRF analysis of snow and plant tissues can be used to carry out a timely and reliable environmental assessment of an urban territory.     

微波消解-石墨炉原子吸收光谱法测定菜籽及饼粕中铅和镉

目前菜籽及饼粕的综合利用越来越受到人们的重视,同时重金属的污染问题也日益引起人们广泛的关注,因此测定菜籽及饼粕中铅和镉的含量具有十分重要的意义。文章研究了微波消解溶剂、微波时间和压力对样品消解效果的影响,优化了石墨炉原子吸收光谱法测定条件,建立了一种快速检测菜籽及饼粕中铅、镉含量的有效方法。研究表明,铅、镉的检出限分别为2.172 μg·L-1(54.30 ng·g-1)、0.243 μg·L-1(6.075 ng·g-1),其线性范围分别为0～100 μg·L-1,0～8 μg·L-1;样品测定回收率在80.8%～110.7%之间,RSD小于5.3%。该法具有检出限低、灵敏度高、快速、准确的特点,用于实际样品测定的结果令人满意。     

ICP-AES法同时测定陶瓷制品铅、镉、铬、钴的溶出量

采用ICP AES法同时测定陶瓷制品铅、镉、铬和钴的溶出量 ,并对 4 %醋酸溶液中仪器入射功率的影响、分析谱线的选择和背景校正及共存元素的干扰等因素进行详细的研究。方法检出限 :铅 6 8μg·L-1;镉 0 18μg·L-1;铬 0 6 1μg·L-1;钴 1 0 μg·L-1。加标回收率为 98%～ 10 4 % ,相对标准偏差为 0 2 7%～1 2 4 %。该法简便快速 ,具有良好的精密度和准确度 ,适用于进出口陶瓷制品的日常检验     

鸡精和味精中铅、镉含量的测定

采用原子吸收法测定了鸡精和味精中污染元素铅、镉的含量。结果表明,不同品牌的鸡精和味精所含铅、镉的量不同。该方法简便、快速、准确、实用。测定的线性范围为铅0.00～10.00 μg·mL-1,镉0.00～4.00 μg·mL-1。铅和镉的精密度试验的相对标准偏差分别为3.15%和4.26%,并进行了回收实验,回收率铅在96.7%～102.1%,镉在91.9%～107.6%之间。     

Variations of Lead Isotopes and Airborne Particulate Concentrations From the Kozani Basin,West Macedonia,Greece

Abstract

The spread and variation in ²⁰⁶Pb/²⁰⁷Pb ratios make Pb isotopes a powerful tool when it comes to detecting trends in airborne particulates originating mainly from power plants. This study was conducted to determine the source of pollution in Kozani area, an affected industrial area. Lead isotopic ratios of air filters under certain meteorological conditions were compared to Pb isotope analyses sampled from lignite mines, but also to Pb isotope analyses of cultivations in soil originating from the reclamation of old abandoned lignite-mines. The particles taken into consideration have an aerodynamic diameter less than 10 μm (PM10). The measurements were carried out in a central part of the town of Kozani, West Macedonia, for one year observation period. The lead isotope values of air filters and of wheat in the Kozani area are between the values of lignite Pb and of Greek gasoline.     

Variations of lead isotopes and airborne particulate concentrations from the Kozani basin,West Macedonia,Greece

The spread and variation in 206Pb/207Pb ratios make Pb isotopes a powerful tool when it comes to detecting trends in airborne particulates originating mainly from power plants. This study was conducted to determine the source of pollution in Kozani area, an affected industrial area. Lead isotopic ratios of air filters under certain meteorological conditions were compared to Pb isotope analyses sampled from lignite mines, but also to Pb isotope analyses of cultivations in soil originating from the reclamation of old abandoned lignite-mines. The particles taken into consideration have an aerodynamic diameter less than 10 microm (PM10). The measurements were carried out in a central part of the town of Kozani, West Macedonia, for one year observation period. The lead isotope values of air filters and of wheat in the Kozani area are between the values of lignite Pb and of Greek gasoline.     

Radioisotope‐induced EDXRF investigation of elemental uptake in cauliflower grown at MSW‐contaminated site

A ¹⁰⁹Cd radioisotope‐induced energy dispersive X‐ray fluorescence (EDXRF) study has been performed on samples of cauliflower consisting of the flower, the leaves and the associated root soil. The cauliflowers are collected from farms near the main dumping site of municipal solid waste (MSW) in the city of Kolkata, India, and also from uncontaminated farms about 50 km away from the city. The systematic investigation is primarily aimed at achieving two correlated objectives. Firstly, a unified calibration approach is undertaken for the study tool viz., EDXRF spectrometer, through the use of same instrumental scattering constants for quantification in widely differing matrices like soil and plant. Quality control was done by quantitative reproduction of National Institute of Standards and Technology–Standard Reference Materials (NIST–SRMs). Subsequently, the second objective is to comparatively study elemental uptake in the cauliflower samples from contaminated and uncontaminated farms using the same calibration. This study suggests that the elemental concentrations in the root soils and leaves of the samples vary from farm to farm, whereby the concentrations of Cu, Zn and Pb in root soils of MSW‐contaminated farms are higher by almost an order of magnitude compared to uncontaminated farms. But the most notable feature of this study is the strikingly similar elemental concentrations in the edible flower part of all samples irrespective of the soil type. Plots of the ratio of concentrations of elements in leaf to soil and in flower to leaf, observed from the present EDXRF study suggests that a preferential uptake of elements takes place at different stages. Copyright © 2010 John Wiley & Sons, Ltd.     

高压密封微波消解-ICP-AES法测定五种蒙药中无机元素

采用HNO3-HClO4消解体系分别对额日敦-乌日勒、德都红花七味丸、通拉嘎-5、乌珠目-7、给旺-9等五种蒙药样品进行高压微波消解制样,利用电感耦合等离子体原子发射光谱法(ICP-AES)同时测定了镁、铝、钙、铬、锰、铁、钴、镍、铜、锌、砷、硒、锶、钼、银、镉和铅等17种无机元素的含量。通过添加标准回收实验,回收率均在97.25%~106.35%之间,验证了分析数据的可靠性。所有元素测定结果的相对标准偏差均小于3.3%,具有良好的准确度和精密度。实验结果表明,其中常量元素Ca,Mg和Fe,Mn,Zn,Cu的含量较高,测定结果可为开发研制蒙药新制剂、研制蒙药的质量控制标准和提高蒙药药效提供理论依据。     

Pb2+印迹丙烯酸-co-苯乙烯的制备及其吸附性的FAAS法分析

以丙烯酸为功能单体、苯乙烯为骨架单体、Pb2+为模板离子、采用无皂乳液聚合法合成铅离子印迹共聚物(Pb(Ⅱ)-ⅡPs)并采用紫外光谱、傅里叶变换红外光谱和扫描电镜对Pb(Ⅱ)-ⅡPs和非印迹聚合物(NIPs)的表面形貌和结构进行表征.以火焰原子吸收光谱法(FAAS)为检测手段,研究了Pb-ⅡPs对Pb2+的吸附和选择识...     

Energy-dispersive X-ray fluorescence study of elemental uptake in cauliflower

A ¹⁰⁹Cd radioisotope-induced energy-dispersive X-ray fluorescence (EDXRF) study has been performed on samples of cauliflower consisting of the flower, the leaves and the associated root soil. The cauliflowers were collected from farms near the main dumping site of municipal solid waste in the city of Kolkata, India and also from uncontaminated farms about 50 km away from the city. A unified calibration approach was undertaken for the elemental analysis of the samples of widely varying matrices. The present study suggests that the elemental concentrations in the root soils and leaves of the samples vary from farm to farm, whereby the concentrations of Cu, Zn and Pb in root soils of MSW-contaminated farms are higher by almost an order of magnitude compared to uncontaminated farms. But, the most notable feature of this study is the strikingly similar elemental concentrations in the edible flower part of all samples irrespective of the type of soil.     

多壁碳纳米管/铋膜修饰电极示差脉冲溶出伏安法测定水中镉和铅

制备多壁碳纳米管/壳聚糖纳米复合物修饰玻碳电极,用于同位镀铋膜法连续测定水中镉和铅离子的含量.将多壁碳纳米管分散在壳聚糖溶液中,滴涂在玻碳电极表面制得修饰电极;在含铋的溶液中,采用示差脉冲溶出伏安法测定了镉、铅离子的浓度;考察了沉积电位、富集时间对溶出电流的影响.在优化的实验条件下,对浓度在0-0.2μmol/L范围内...     

微型柱现场预富集流动注射火焰原子吸收测定环境水样中的铅和镉

文章以负载8-羟基喹啉(8-HQ, Oxine)、二乙基二硫代氨基甲酸盐(DDTC)和吡咯啶二硫代氨基甲酸铵(APDC)三种螯合剂的活性炭(AC)为微型柱的吸附材料,采用微型柱现场采样 (MFS)分析技术实现了连续现场富集环境水样中的痕量Pb和Cd,并在实验室中采用流动注射(FI) -火焰原子吸收(FAAS)联用技术对吸附柱中富集的Pb和Cd进行测定。该方法用于水中微量元素(GBW—08608)和南湖水样中Pb和Cd的测定均获得了满意的结果。10 mL富集的检出限(3σ)Pb：1.58 μg·L-1;Cd：0.062 μg·L-1 ,相对标准偏差Pb：1.62%;Cd：1.96%。     

苦菜的不同部位中13种金属元素含量的分析测定

用火焰原子吸收法测定了苦菜的不同部位(根,茎,叶,花)中矿物元素(Ca, Mg, K, Na, Cu, Zn, Mn, Cr, Co, Ni, Fe, Pb和Cd)的含量,并对结果进行了分析比较。苦菜中13种金属元素在各部位中的加合量(μg·g-1)由高到低的顺序依次为：叶(77 213.72)>花(47 927.15)> 杆 (42 280.99 )>根(28 131.18)。人体必需的生理上较重要的微量元素Zn, Fe, Mn, Cu等含量均较高。另外, 样品中亦检出微量有毒元素铅和镉。