微波消解法测定生物燃料样品中铝钙铬钾镁锰磷锌

生物燃料来源于可再生的有机材料。绝大多数的生物质材料是植物产品或废物,如粮食、油料作物、木头、木板、树皮或碎屑。这些生物质材料由于可以作为替代能源而变得越来越重要,所以人们迫切需要一个能准确测定生物燃料中的主次量元素的分析方法。生物燃料中Al、K、Na、Ca、Mg、Fe和P等主要灰分形成元素,与生物质热工艺转化过程中的灰融、沉积形成和腐蚀等问题有关。而As、Cd、Co、Cu、Cr、Hg、Mo、Mn、Ni、Pb、V、Zn等次量元素由于大气排放问题也十分重要。虽然现在也有一些方法来分析固体燃料中的主量和次量元素;但是测量的精度仍不理想。其中的一个关键问题是这些生物质燃料中的灰分形成元素具有非常复杂     

密闭微波消解法测定钢铁样品中的硼

微波消解是对钢铁试样进行快速分解的非常有效的途径。密闭式压力反应罐可防止酸的蒸发和挥发性元素的损失,并且微波消解加热快速,钢样可以用最少体积的酸溶解。\r\n本文对用微波消解ICP-OES法测定硼的分析精度、再现性、重复性和准确度等进行了考察和优化,并且对记忆效应、光谱干扰、漂移补偿、离子体参数、回收率、内标和外标的使用及依据国际公认标准的可溯源性进行了研究。\r\n本项工作研究的目的是根据《EURACHEM/CITAC量化分析测量不确定度指南》的要求开发一种经验证的测定方法。根据该指南,本文对认证分析过程及获得主要影响因素进行了相关统计。\r\n对于含1.80％（质量分数）硼的钢的分析,其总不确定度被评定为0.02％ (标准偏差),相当于相对标准偏差（RSD）为1.1%。相关的研究表明,在整个分析方法的不确定度中,来自于样品制备步骤的贡献远远小于ICP-OES仪器不稳定性的影响。     

ICP-OES法测定煤样中磷、铜、铅、锌、镉、铬、镍、钴等元素

采用硝酸—氢氟酸—高氟酸混合体系,微波消解样品,用ICP-OES法测定煤样中微量元素P、Cu、Pb、Zn、Cr、Dd、Ni、Co,快速简便、准确度高。     

全反射X射线荧光光谱法同时测定复混肥料中钒铬锰铁镍铜锌铅

样品经硝酸微波消解,以镓为内标,采用全反射X射线荧光光谱法(TXRF)同时测定复混肥料中的钒、铬、锰、铁、镍、铜、锌、铅,方法检出限从铅的1.0μg/g到钒的7.0μg/g,精密度(RSD)铬为2.5%,铅为16%,除铅以外,其余元素的RSD均小于10%;方法回收率为80%～120%,Pb的回收率略低主要是由于化肥中As Kα谱线对Pb Lα谱线的干扰导致测定结果偏低。用TXRF和电感耦合等离子体发射光谱法(ICP-AES)测定不同复混肥料中各元素的含量,经统计检验,两种方法测定结果在95%置信区间内无显著性差异。对于金属元素含量较高的样品,TXRF法测定结果的相对标准偏差小于ICP-AES法。对于不同的复混肥料,在微量、痕量元素检测范围内,TXRF法具有较高的准确度和适用性,仪器使用和维护成本低,方法快速准确。     

Comparative study of As,Cd, Cu,Cr, Mg,Mn, Ni,Pb and Zn concentrations between sediment and water from estuary and port

The contents of As, Cd, Cu, Cr, Mg, Mn, Ni, Pb and Zn have been determined in sediment and water samples from Valle de las Garzas estuary and Port Manzanillo (Colima, Mexico) using ICP-AES. The concentrations of these elements were used for a comparative study to determine the distribution of heavy metals and to evaluate which elements reflect natural or anthropogenic backgrounds. For this purpose, seven sampling points were selected: Four of them correspond to the lagoon, and three were situated in the port. Statistical analysis of the mineral content was assessed. Initially, data comparison was assessed by statistical tests for each variable. Principal component analysis was then applied considering the influence of all variables at the same time by obtaining the distribution of samples according to their scores in the principal component space. In this way, four studies were carried out: (1) study of sediments collected during the dry season; (2) study of sediments collected during the rainy season; (3) comparative study between sediments from rainy and dry season; and (4) study of water composition collected during rainy season. From the results of the performed analyses, it can be concluded that metals distribution pattern reflected natural and anthropogenic backgrounds (e.g., sediments from the lagoon, situated at the beginning of the rain channel, presented high contents of Zn and Cu, perhaps related to anthropogenic activities or the influence of igneous sediments).     

The distribution of Co,Cr, Cu,Fe, Mn,Ni and Zn in Framvaren,a Norwegian anoxic fjord

Sediments collected from a Norwegian anoxic fjord have been analyzed for Fe, Co, Cu, Mn, Ni and Zn. With the exception of Zn, the dominant factors effecting their distributions are the mineralogy of the land-derived lithogenic material and the abundance of organic matter.     

手持式X射线荧光光谱仪测定富钴结壳样品中锰铁钴镍铜锌

便携式X射线荧光光谱仪可以快速进行多元素实时分析,在富钴结壳资源勘查中有广阔的应用前景,但是现有仪器的分辨率和稳定性有待进一步提高,特别是现场原位分析法的应用有待研究。本文针对富钴结壳中目标元素含量相对较高的特点,采用松散粉末法制样,建立了手持式X射线荧光光谱仪快速测定太平洋富钴结壳样品中Mn、Fe、Co、Ni、Cu和Zn的分析方法。该方法用多金属结核和富钴结壳国家标准物质进行验证,测定值的相对标准偏差(RSD)在0.2%~3.0%之间,测定值与标准值的相对误差为92.9%~107.6%。样品现场分析和实验室分析的数据对比表明,除了低含量Cu略有超差外,Mn、Fe、Co、Ni、Zn和品位均无超差,完全满足该类矿产资源勘查规程的要求。本法简单、高效,适用于对野外富钴结壳资源作出快速的初步评价。     

ICP-MS测定土壤中的As、Cr、Pb、Se、Cu和Zn

本文用电感耦合等离子质谱法(ICP-MS)测定了土壤的As、Cr、Pb、Se、Cu和Zn6种微量元素的质量分数,以In作为内标进行基体效应的补偿,方法快速灵敏,回收率为92.4%～106.8%,相对标准偏差小于5.0%,结果达到国家标准要求。     

无高氯酸常压酸溶-ICP-MS法同时测定土壤中的As、Cd、Pb、Cr、Zn、Cu、Ni

采用无高氯酸常压酸溶分解土壤样品,利用等离子体质谱法可以1次溶矿测定As、Cd、Pb、Cr、Zn、Cu、Ni 7个重金属元素,具有较高的分析效率、较好的分析质量、较低的分析成本。实验表明,试样溶液中氯的含量对分析元素信号有较大影响。采用硝酸-氢氟酸-硫酸-过氧化氢分解样品以避免引入氯离子,从而能有效避免Cr、As元素在样品分解过程中的损失和氯离子产生的质谱干扰。Cd的测定需采用干扰校正公式扣除Sn的干扰。对于As元素,若试样溶液中不含或仅含微量的氯离子,采用标准模式测定即可得到理想的分析结果,否则必须采用CCT模式进行测定。除As以外的其他元素不论在标准模式或CCT模式下均能得到理想的分析结果。     

阴离子交换色谱分离和测定微量单矿物方铅矿和闪锌矿中铜、铅、锌、银、铋、镉、锰、钴和镍等元素

微量单矿物方铅矿和闪锌矿中主体元素和痕量元素的多项分析,作者根据金属元素在阴离子交换树脂上与在盐酸、氢溴酸、硝酸、硫酸溶液之间的行为差别,试验了用阴离子交换色谱分离的条件,选用不同浓度的盐酸溶液洗提铜、钴、镍、锰、铅和银;氢溴酸溶液洗提锌;硝酸溶液洗提镉;最后用硫酸溶液洗提铋。本文所拟定的分析流程简便,试用于微量单矿物方铅矿和闪锌矿中九个元素的测定,效果较好。 实验部分 一、主要试剂     

Delivery of Trace Metals (Al,Fe, Mn,V, Co,Ni, Cu,Cd, Ag,Pb) from the Trinity River Watershed Towards the Ocean

The Trinity River (Texas, USA) contains in its watershed 23 different reservoir lakes, the largest one being Lake Livingston situated in the lower Trinity River watershed and two potentially polluting metroplexes, Dallas and Houston. In order to determine fluxes of nutrients and trace metals to Galveston Bay, a survey that included 24 discreet samples collected over a year and at various stages of discharge was carried out during 2000–2001. Geochemical (i.e., sorption by Fe oxyhydroxides), biological (i.e., seasonal uptake by sinking algae in Lake Livingston), and hydrological (i.e., dilution effects by increasing flow rates) controls were found to be mainly responsible for variations in dissolved trace metal concentrations rather than pollution sources. The Trinity River loads of suspended sediments and pollutant trace metals entering Galveston Bay at Anahuac were <20% of those reaching Lake Livingston, and only a few percent of the total upstream trace metal load is entering the Gulf of Mexico. Thus, during the transit through the 23 man-made lakes and an estuary, >96% of the pollutant trace metal load is lost to sediments.     

原子吸收法连续测定铋及氧化铋中铜铅铁镉镍

HNO3分解样品后,直接用火焰原子吸收法测定铋及氧化铋中铜、铅、铁、锡、镍。方法的检出限分别为Cu 0．22μg／g,Pb1．5μg／g,Fe0．39μg／g,Cd0．11μg／g,Ni0．34μg／g。与国标方法进行比较,分析结果基本一致,精密度试验,各元素的RSD(n＝6)≤5．2％。