微波消解技术在沉积物样品重金属元素分析中的应用

通过利用微波消解—原子吸收法测定标准河流沉积物样品中重金属元素Cu、Ni、Zn、Mn的含量，优化了微波消解的工作条件，并与电热板消解法进行了比对试验。结果表明，微波消解法与传统方法相比无显著性差异，且高效快速、试剂消耗量少、节约能源。     

微波消解法测定有机磷农药废水中的总磷

应用微波消解技术进行了农药废水测定总磷的研究，考察微波消解方法的消解时间、功率对消解的影响，并将该方法与GB11893—1989《钼酸铵分光光度法》中规定的消解方法进行比较．实验证明，微波消解法操作简便，测定结果准确可靠．     

黄河甘宁蒙段表层沉积物中总磷3种提取方法的比较

通过微波消解法、标准测试方法(SMT)和碱熔法分别测定了水系沉积物成分分析标准物质GBW07307a(GSD-7a)中的总磷(TP)含量,并分别采用3种方法对采集于黄河流域甘宁蒙段表层沉积物样品进行TP含量和样品加标回收率的测定。结果表明:测定标准物质的相对误差绝对值:微波消解法碱熔法SMT法;变异系数:微波消解法碱熔法SMT法。同时,微波消解法提取的表层沉积物TP含量的范围为634.3~909.2μg/g;SMT法TP含量的范围为627.1~889.5μg/g;碱熔法TP含量的范围为559.1~784.8μg/g。微波消解法的测定结果相对偏高,SMT法的测定结果相对偏低。样品加标回收率平均值:微波消解法SMT法碱熔法;变异系数:微波消解法碱熔法SMT法。综合测定标准物质中TP含量以及样品加标回收率实验结果的准确度和精密度,对于黄河甘宁蒙段表层沉积物,使用SMT法提取TP较优于微波消解法和碱熔法。     

微波消解预处理测定水和废水中总磷

提出一种用微波消解技术作为测定水和废水中总磷的预处理方法，这种消解方法只需10min即可，比用常规的高温高压消解法节省三分之一时间。用这身份种消解法对标样、地表水、海水、生活污水和工业废水样品进行了对比测定，所得结果经统计检验，两方法之间无显著性差异。对微波消解法的精密度和准确度进行了验证。     

微波消解—火焰原子吸收法测定废气中铅的方法研究

分别使用微波消解方法和传统的酸煮法对含铅滤筒进行前处理,采用火焰原子吸收法测定废气中的铅.结果表明,微波消解法具有消耗试剂少、效率高、速度快、结果准确等特点.     

微波消解-原子荧光法同时测定TSP中砷和汞

通过比较不同滤膜的透气效率和空白值来选择采样滤膜,探讨了不同消解方法的前处理效果,进行精密性、准确性及实际样品测试等条件实验,建立了微波消解-原子荧光法同时测定大气环境TSP中砷和汞的方法。结果表明,过氯乙烯滤膜透气性好,空白值低且稳定,微波消解能使样品消解更完全,精密度好,回收率高,尤其汞的损失少。     

微波消解-火焰原子吸收光谱法测定芦苇笋中的镉

采用密闭微波消解-火焰原子吸收光谱法对洞庭湖区芦苇笋中的镉进行了测定.结果表明,密闭微波消解是一种非常有效的植物样品前处理方法,对国家标准物质灌木枝叶的测定结果与推荐值吻合,表明该方法准确可靠.     

微波消解和ASD消解ICP-MS测定土壤中重金属元素的比较

采用微波消解和ASD消解2种消解方式对不同土壤样品进行消解,ICP-MS测定其中重金属含量。微波和ASD2种消解方式均能够较好地提取土壤中的Cr、Co、Ni、Mn和V元素,实验结果的相对误差和相对标准偏差均≤10%,符合实验分析的要求。微波消解精密度优于ASD,可作为优先选择的前处理方法。     

石墨炉原子吸收光谱法测定农产品中痕量铍

采用石墨炉原子吸收光谱法测定农产品中痕量铍，比较了微波消解和电热板消解两种前处理方法，选择了基体改良剂。方法在0μg／L—4.00μg／L范围内线性良好，微波消解法和电热板消解法的检出限分别为0.002mg／kg和0.0002mg／kg，标样平行测定的RSD为2.4％—4.1％，农产品加标回收率为80.0％—95.0％。     

固体废物的不同前处理分析测试对比

针对固体废物的分布不均匀性、组分复杂、形态多变等特性,以及我国的固体废物环境管理和监测框架体系,文章使用硫酸硝酸法、醋酸缓冲溶液法、水平振荡法对固体废物进行浸出前处理,同时使用微波消解、王水浴进行全量消解。使用双道原子荧光分光光度计测试浸出液和全量消解液中汞和砷元素,对比分析不同的处理方法得出不同的结果。     

Development of a hybrid pollution index for heavy metals in marine and estuarine sediments

Heavy metal pollution of sediments is a growing concern in most parts of the world, and numerous studies focussed on identifying contaminated sediments by using a range of digestion methods and pollution indices to estimate sediment contamination have been described in the literature. The current work provides a critical review of the more commonly used sediment digestion methods and identifies that weak acid digestion is more likely to provide guidance on elements that are likely to be bioavailable than other traditional methods of digestion. This work also reviews common pollution indices and identifies the Nemerow Pollution Index as the most appropriate method for establishing overall sediment quality. Consequently, a modified Pollution Index that can lead to a more reliable understanding of whole sediment quality is proposed. This modified pollution index is then tested against a number of existing studies and demonstrated to give a reliable and rapid estimate of sediment contamination and quality.     

地表水总氮总磷联合消解测定方法的研究

针对目前我国文献中总氮(TN)和总磷(TP)联合消解测定的试验条件差异较大的问题,通过与标准方法对比。建立了一种地表水总氮和总磷联合消解测定的方法。当水样量为25ml时,过硫酸钾和氢氧化钠的加入质量分别为0.5g和0．12g,可同时满足2个项目的消解要求。该方法操作简单快速,可应用于地表水的检测。     

土壤重(类)金属消解方法的研究进展

综述了目前国内外土壤重(类)金属的消解方法及相关标准,分析了各种方法的优缺点。指出传统的电热板消解法已逐渐被淘汰,微波消解法应用广泛却存在一定的局限性,全自动石墨消解法自动化程度高,适合大批量样品前处理,应用前景良好。提出相对于加入氢氟酸的混酸消解法获得的土壤重(类)金属全量,王水消解法获得的土壤重(类)金属总环境有效态与生物有效性相关性更好,研究者可根据需要选择合适的消解方法。     

底质样品微波消解总磷测定研究

使用硫酸_高氯酸在微波消解系统消解 ,以钼锑抗比色法测定底质中的总磷 ,通过实验确定最佳消解及分析条件。结果表明 ,该方法快速简便并有较高准确度、精密度和较低的检测限 ,值得推广和应用。     

Determination of Pb and Cd in road dusts over the period in which Pb was removed from petrol in the UK

It is commonly agreed that automobile exhaust has been the most important source of Pb pollution in urban areas, and that Cd may come from wear and tear of tyres. This study evaluates the fall in Pb concentrations in road dusts in Manchester as a consequence of the removal of Pb from petrol in January 2000. In the work presented here a slurry graphite furnace atomic absorption methodology for the determination of Pb and Cd in road dusts has been developed and is compared with an acid digestion method in terms of efficiency. The reproducibility and accuracy of the results obtained by acid digestion and the slurry method have been studied and a certified reference material CRM 038 was analysed to confirm the reliability of the proposed methods. Different factors were evaluated throughout this work including: (i) the effect of traffic density on Pb and Cd levels in road dust samples collected weekly during the period of May 1999 until September 2000; (ii) comparison between the Pb and Cd levels in a busy road and a residential street; (iii) the effect of distance from the source on Pb and Cd levels; The results of these experiments show a reduction in Pb levels over the sampling period. The relationship between road dust particle size and Pb and Cd concentration was also investigated in the 4-250 microns size range using the slurry method, showing that there is a relationship between metal concentration and particle size; the highest concentrations being for the smallest particle size.     

Trace metal levels and some chemical parameters in herby cheese collected from south eastern Anatolia-Turkey

Due to the consumption of the herby cheese in south eastern Anatolia-Turkey is at high ratio, chemical parameters such as dry matter, pH, acidity, aCl, protein, fat and trace metal contents in 50 different herby cheeses produced at this region have been determined in the presented study. The content of lead, copper, cobalt, nickel, chromium, cadmium, and iron have been analyzed by flame atomic absorption spectrometer in air/acetylene flame after combination ash digestion method and wet digestion method. The mean concentration of lead, copper, cobalt, nickel, chromium and cadmium in our samples are higher than literature values except iron.     

测定废水重金属样品的高压蒸汽消解方法

本文采用正交实验方法，用自己研制的“自控式高压蒸汽消解器”，详细研究了测定废水重金属，样品的最佳消解条件，并用于实际废水样的消解和重金属的测定，准确度和精密度均优于传统的敞口消解法，并具有试剂用量少、时间短、不受污染、操作简单，批处理样品量大等优点，可作为测定废水中重金属，样品的常规消解方法。     

土壤重金属含量测定不同消解方法比较研究

消解是影响土壤重金属测定结果准确性的关键步骤.比较电热板消解、微波消解和全自动石墨消解3种消解方法的操作流程,同时对不同类型土壤样品中Cu、Zn、Pb、Cd、Cr、Ni 6种元素含量进行对比测定,结果表明,电热板消解设备简单,但步骤繁锁,操作不当易造成组分损失；微波消解速度快,测定结果精密性和准确性较好,但仍需人工赶酸程序且罐位少,不适合大批量样品分析；全自动石墨消解不仅测定结果精密性和准确性较好,而且自动化程度高,可实现无人值守,大大节省人力,尤其适合大批量样品的分析.     

Iodide-assisted total lead measurement and determination of different lead fractions in drinking water samples

Lead and its compounds are toxic and can harm human health, especially the intelligence development in children. Accurate measurement of total lead present in drinking water is crucial in determining the extent of lead contamination and human exposure due to drinking water consumption. The USEPA method for total lead measurement (no. 200.8) is often used to analyze lead levels in drinking water. However, in the presence of high concentration of the tetravalent lead corrosion product PbO(2), the USEPA method was not able to fully recover particulate lead due to incomplete dissolution of PbO(2) particles during strong acid digestion. In this study, a new procedure that integrates membrane separation, iodometric PbO(2) measurement, strong acid digestion and ICP-MS measurement was proposed and evaluated for accurate total lead measurement and quantification of different lead fractions including soluble Pb(2+), particulate Pb(II) carbonate and PbO(2) in drinking water samples. The proposed procedure was evaluated using drinking water reconstituted with spiked Pb(2+), spiked particulate Pb(II) carbonate and in situ formed or spiked PbO(2). Recovery tests showed that the proposed procedure and the USEPA method can achieve 93-112% and 86-103% recoveries respectively for samples containing low PbO(2) concentrations (0.018-0.076 mg Pb per L). For samples containing higher concentrations of PbO(2) (0.089-1.316 mg Pb per L), the USEPA method failed to meet the recovery requirement for total lead (85-115%) while the proposed method can achieve satisfactory recoveries (91-111%) and differentiate the soluble Pb(2+), particulate Pb(II) carbonate and PbO(2).     

两种消解法测定沉积物总磷的对比

通过过硫酸钾消解法与HClO₄-H₂SO₄消解法对土壤和水系沉积物的标准物质,以及三峡水库沉积物未知样品中的总磷含量进行测定,并对检测结果进行对比,分析过硫酸钾消解法测定沉积物总磷的可行性。结果表明,在标准样品中,HClO₄-H₂SO₄消解法的检测结果是标准值的83%~100%,并且所有结果均在其不确定度范围之内;过硫酸钾消解法的检测结果仅达到标准值的19%~42%,超出其不确定度范围,不能作为有效数据。在未知样品中,过硫酸钾消解法检测结果也远低于HClO₄-H₂SO₄消解法检测结果,只达到后者的32%~52%。由此可见,过硫酸钾消解法测定沉积物或土壤中总磷,仍需要进一步的研究,以达到符合实际的检测结果。