能量色散X射线荧光光谱法测定土壤和沉积物中稀土元素

建立了偏振能量色散X射线荧光光谱法测定土壤和沉积物中稀土元素的方法,该方法较传统的方法具有前处理简单、测量自动化程度高、灵敏度高和检出限低(检出限范围为0.05~2.80 mg/kg)等优点。对土壤和沉积物标准物质的测定结果表明:测定结果与认定值能较好吻合,相对标准偏差范围为0.2%~9.4%,能满足测试的需求。分别用该方法和电感耦合等离子体质谱法对实际样品进行测定,2种方法的测定结果有较好的一致性,表明该方法测定结果准确可靠,可用于实际样品的测定。     

土壤中18种元素的ICP-AES同时测定

本文对ICPQ—1000型等离子发射光谱仪测定土壤中18种元素的条件进行了研究、确定了最佳工作条件。该方法已用于40种不同类型土壤的近千个样品的实测中,并经多种方式考查,证明分析结果可靠。     

加速溶剂萃取-凝胶净化色谱-气相色谱质谱法测定农用地土壤中有机氯农药方法研究

通过对加速溶剂萃取、平行蒸发及净化方法等环节的优化实验,建立了加速溶剂萃取-凝胶净化色谱-气相色谱质谱法测定农用地土壤中23种有机氯农药的检测方法。结果表明,方法检出限为0.0034~0.0052 mg/kg;对化合物质量分数为0.25 mg/kg的土壤加标样品进行平行实验,回收率为82.0%~93.7%;测定结果的相对标准偏差（RSD）≤8.7%。对土壤有证标准质控样品进行分析,测定结果均在验收范围之内。该方法准确可靠,灵敏度较高,样品净化效果较好,能够满足农用地土壤中有机氯农药残留痕量分析的要求。     

土壤重金属监测过程及其质量控制

重点探讨了土壤中典型重金属含量监测过程中样品制备、含水率、预处理等因素对分析结果的影响。实验结果表明,充分风干土壤的含水率在2%～3%左右,200目土壤颗粒度可满足分析精度的要求。硝酸-氢氟酸-高氯酸的多元混酸消解体系可实现对土壤重金属的充分溶解,对标准土壤样品中各元素的回收率可达84%～98%。批次内平行样品以及批次间质控样品各元素的相对标准偏差大都小于10%,符合《土壤环境监测技术规范》的要求,表明该研究建立的系统土壤重金属检测方法结果准确可靠。     

微波消解-分光光度法测定土壤中的全硼

研究了分光光度法测定土壤中的全硼时样品的微波消解方法.建立了合理的分析步骤.进行了微波消解条件的选择及测定结果精密度、准确度实验.实验结果为:消解完全仅需25min,相对标准偏差7.6%,其方法的加标回收率为98.4%～112%.结果表明,微波消解-分光光度法测定土壤中的全硼是一种快速、准确且低环境污染的方法.     

基质固相分散-快速溶剂萃取-GC/MS法同时测定土壤中有机氯农药和多环芳烃

建立了基质固相分散-ASE提取-GC/MS法同时测定土壤中8种有机氯农药和16种多环芳烃的方法。对方法的线性、检出限、精密度、回收率及土壤质控样品进行了分析,结果表明,8种有机氯农药和16种多环芳烃线性良好,相关系数为0.997 5～0.999 8,方法检出限为0.39～1.57μg/kg,空白加标样品的相对标准偏差小于20%,实际土壤样品加标回收率为60.6%～125%,土壤质控样品结果均在范围内。该方法能够满足土壤中8种有机氯农药和16种多环芳烃的检测要求。     

加速溶剂萃取-气相色谱质谱法同时测定土壤及沉积物中34种有机氯农药及18种多氯联苯类化合物

建立了加速溶剂萃取-气相色谱质谱法同时测定34种有机氯农药(OCPs)和18种多氯联苯类化合物(PCBs)的方法。当取样量为10. 0 g时,52种有机化合物的检出限为0. 03～0. 29μg/kg,以空白样品为基体进行加标回收试验,平均回收率为44. 7%～123. 0%,相对标准偏差(RSD,n=7)为1. 8%～21. 5%。该方法灵敏度高,实现了低浓度有机化合物的定量分析,分析结果准确可靠,满足土壤和沉积物中34种有机氯农药和18种多氯联苯类化合物分析的要求。     

微波消解-ICP-MS测定土壤和底泥中的12种金属元素

以20.0μg/L铟作内标,采用硝酸-氢氟酸-过氧化氢体系微波消解,ICP-MS(电感耦合等离子体质谱法)同时测定土壤和底泥中的12种金属元素,各元素方法检出限为0.003～0.2μg/g,相对标准偏差小于6.1%,土壤标准样品的测定值与标准值吻合。方法简便快捷,灵敏度高,重现性好,是分析大批量土壤和底泥样品中多元素的可靠、高效方法。     

悬浮液进样石墨炉原子吸收法直接测定土壤、底泥中的铅、镓、钴、镍

介绍一种悬浮液进样直接测定土壤、底泥中多种微量金属元素的快速分析方法。基体改进剂的使用，适宜的原子化温度的选择，使用水相标准溶液作校准曲线成为可能．对标准作品的测定证明了此方法的精密度和准确度较好，适合于常规环境样品分析．     

电感耦合等离子体法(ICP-MS)测定地表水12种稀土元素

建立电感耦合等离子体质谱法(ICP-MS)测定地表水中镨、钕、钐、铕、钆、铽、镝、钬、铒、铥、镱、镥12种稀土元素的方法。地表水样品通过0.45μm滤膜过滤后,试液直接用ICP-MS同时测定上述12种重金属元素。以铑和铼作为内标物质,校正响应信号的变化,消除基体效应;选择适当的待测元素同位素克服了质谱干扰;确定了最佳测定条件。结果表明,12种稀土元素的检出限为0.01～0.02μg/L;相关系数r0.999 0;实际样品加标回收率为91.5%～106%;相对标准偏差为0.26%～1.09%。该方法简便、快速、准确,可应用于地表水中微量重金属元素的测定。     

土壤重金属元素检测国际实验室比对研究

IERM和CNAS合作组织开展了亚太实验室合作组织(APLAC)能力验证计划"APLAC T066土壤重金属元素检测",其目的是评价参加实验室定量分析土壤重金属元素总量的能力。研究所用的能力验证样品为IERM研制的土壤标准样品。结果表明,参加实验室检测土壤砷、铜、汞、镍、铅和锌的结果满意率分别为85.7%、95.8%、77.1%、83.3%、93.5%和91.7%。样品消解过程加入氢氟酸时,铅和锌的检测结果与标准值更加接近,说明检测土壤重金属元素总量时氢氟酸的加入非常关键。文章还对比对实验室结果评价的统计方法进行了探讨。     

土壤背景值数据差异的来源分析及土壤类型对背景值的影响

本文阐述了在我国共８６０多个土壤样品、４１种土类中的４８种元素背景值调查研究中，元素含量差异的来源并估计了各部分来源的差异所占比例；同时采用单因素方差分析法，研究了土壤类型对４８种元素背景值的影响。结果表明，土壤背景值数据的伯差主要来源于样品本身固有的差异；常量元素的采样偏差大于分析测试过程产生的偏差；而微量元素的分析测试偏差大于采样偏差。     

Application of a modified BCR sequential extraction (three-step) procedure for the determination of extractable trace metal contents in a sewage sludge amended soil reference material (CRM 483), complemented by a three-year stability study of acetic acid and EDTA extractable metal content

This paper provides additional data on a sewage sludge amended soil certified reference material, CRM 483, which was certified in 1997 for its EDTA and acetic acid extractable contents of some trace metals, following standardised extraction procedures. The additional work aimed to test the long-term stability of the material and the applicability of an improved version of the BCR three-step sequential extraction procedure on the sewage sludge amended soil (CRM 483). The paper demonstrates the CRM 483 long-term stability for EDTA and acetic acid extractable contents of Cd, Cr, Cu, Ni, Pb and Zn and gives the results (obtained in the framework of an interlaboratory study) for the extractable contents of the same elements in the CRM 483, following the BCR three-step sequential extraction scheme. The aqua regia extractable contents following the ISO 11466 Standard are also given. The data are given as indicative (not certified) values.     

微波消解ICP-MS法测定宣威和富源土壤中的微量元素

建立了微波消解-ICP-MS法测定土壤中32种微量元素的方法。采用氢氟酸-硝酸-过氧化氢体系微波消解,稀释定容后用ICP-MS对溶液进行元素的测定,在优化仪器工作参数后,以双内标铑(Rh)和铼(Re)进行校正。元素检出限为0.01～0.45ng/ml,测定国家标准物质西藏土壤成分分析标准物质GBW 08302中的元素,测定值与标准值或参考值基本一致,用该法测定云南宣威和富源两地24份土壤样品结果表明,该方法快速、简便、准确,适于土壤中多种微量元素的测定。     

富蕴县耕地土壤环境质量现状

通过在富蕴县建立测土配方施肥示范点，开展了耕地土壤环境质量的调查，结果表明：在富蕴县不同地貌部位0 cm~20 cm耕层土壤中，土壤常量元素的分布与微量元素相比差异较大；在山区土壤中，常量元素与微量元素的含量较高，而在戈壁沙漠地带，土壤中常、微量元素的含量均表现为最低水平；土壤pH值为7.5~8.5，适合作物生长；土壤耕层盐分含量相对较低，仅表现为轻盐化土壤类型，占总耕地面积的12.52%。     

Background levels of some major,trace, and rare earth elements in indigenous plant species growing in Norway and the influence of soil acidification,soil parent material,and seasonal variation on these levels

Baseline levels of 43 elements, including major, trace, and rare earth elements (REEs) in several native plant species growing in boreal and alpine areas, are presented. Focus is placed on species metal levels at different soil conditions, temporal variations in plant tissue metal concentrations, and interspecies variation in metal concentrations. Vegetation samples were collected at Sogndal, a pristine site in western Norway, and at Risdalsheia, an acidified site in southernmost Norway. Metal concentrations in the different species sampled in western Norway are compared with relevant literature data from Norway, Finland, and northwest Russia, assumed to represent natural conditions. Except for aluminium (Al) and macronutrients, the levels of metals were generally lower in western Norway than in southern Norway and may be considered close to natural background levels. In southern Norway, the levels of cadmium (Cd) and lead (Pb) in particular appear to be affected by air pollution, either by direct atmospheric supply or through soil acidification. Levels of some elements show considerable variability between as well as within plant species. Calcium (Ca), magnesium (Mg), and potassium (K) are higher in most species at Sogndal compared to Risdalsheia, despite increased extractable concentrations in surface soil in the south, probably attributed to different buffer mechanisms in surface soil. Antagonism on plant uptake is suggested between Ca, Mg, and K on one hand and Al on the other. Tolerance among calcifuges to acid conditions and a particular ability to detoxify or avoid uptake of Al ions are noticeable for Vaccinium vitis-idaea.     

微波消解-氢化物发生原子荧光光度法 测定土壤中的砷

建立了微波消解一氢化物发生原子荧光光度法测定土壤中砷的方法。对微波消解条件进行了优化，用5mL硝酸和2mL过氧化氢的混合酸作消解溶剂，在设定的微波条件下砷提取完全。用5％的盐酸作为反应载流，12g／L硼氢化钾与0．5％氢氧化钠的混合液为还原剂，直接定容后应用HG．AFS测定，并通过测定国家标准参考物质和加标回收实验，对方法进行了验证。实际土壤加标同收率97％～103％。     

Contamination assessment of arsenic and heavy metals in a typical abandoned estuary wetland—a case study of the Yellow River Delta Natural Reserve

Coastal and estuarine areas are often polluted by heavy metals that result from industrial production and agricultural activities. In this study, we investigated the concentration trait and vertical pattern of trace elements, such as As, Cd, Ni, Zn, Pb, Cu, and Cr, and the relationship between those trace elements and the soil properties in coastal wetlands using 28 profiles that were surveyed across the Diaokouhe Nature Reserve (DKHNR). The goal of this study is to investigate profile distribution characteristics of heavy metals in different wetland types and their variations with the soil depth to assess heavy metal pollution using pollution indices and to identify the pollution sources using multivariate analysis and sediment quality guidelines. Principal component analysis, cluster analysis, and pollution level indices were applied to evaluate the contamination conditions due to wetland degradation. The findings indicated that the concentration of trace elements decreased with the soil depth, while Cd increases with soil depth. The As concentrations in reed swamps and Suaeda heteroptera surface layers were slightly higher than those in other land use types. All six heavy metals, i.e., Ni, Cu, As, Zn, Cr, and Pb, were strongly associated with PC1 (positive loading) and could reflect the contribution of natural geological sources of metals into the coastal sediments. PC2 is highly associated with Cd and could represent anthropogenic sources of metal pollution. Most of the heavy metals exhibited significant positive correlations with total concentrations; however, no significant correlations were observed between them and the soil salt and soil organic carbon. Soil organic carbon exhibited a positive linear relationship with Cu, Pb, and Zn in the first soil layer (0–20 cm); As, Cr, Cu, Ni, Pb, and Zn in the second layer (20–40 cm); and As, Cr, Cu, Ni, Pb, and Zn in the third layer (40–60 cm). Soil organic carbon exhibited only a negative correlation with Cd (P?I _geo values), which averaged less than 0 in the three soil layers, this finding indicates that the soils have remained unpolluted by these heavy metals. The mean concentrations of these trace elements were lower than Class I criteria. The degradation wetland restoration suggestions have also been provided in such a way as to restore the reserved flow path of the Yellow River. The results that are associated with trace element contamination would be helpful in providing scientific directions to restore wetlands across the world.