雾化进样石墨炉原子吸收光谱法的研究 Ⅰ.直接雾化进样装置及其性能

介绍一种自行设计和加工的直接雾化石墨炉进样装置的结构、工作原理和操作方法。该装置由微机控制与石墨炉加热程序同步工作,可以实现自动控制和自动测量。对雾化进样石墨炉分析的仪器参数和实验条件进行了研究和选择。结果表明,该装置与石墨炉结合具有自动化程度高、重现性好、样品利用率高和分析速度快等特点。     

塞曼石墨炉原子吸收法直接测定海水中的铜

本文选择酒石酸消除海水基体对铜信号的干扰,用塞曼石墨炉原子吸收法直接测定海水中的铜。从Cu的原子化曲线可知,加入酒石酸后,背景值减小,Cu原子吸收信号增强,且出现时间提前,表明酒石酸是有效的海水基体改进剂。用P.E.Z3030光谱仪测得双蒸水及海水中的元素Cu的特征质量(m。)分别为12.5pg及12.7pg;检测限分别为0.18μg/L和0.19μg/L,表明基体效应已消除,符合海洋监测要求。可用纯Cu标准溶液作校正曲线,以国家海洋局的两个标准海水样品中的Cu评定本法的准确度,相对偏差为0及-4.6%,与经典的经富集后的FAAS法的结果相比,相对偏差在3.0—6.5％范围内。用不同类型的光谱仪测定了30个海水样品,回收率在89—104％范围内。本法操作简便、快速。     

塞曼石墨炉原子吸收法直接测定海水中的铬

海水基体对Cr有增感作用。本文研究了抗坏血酸、柠檬酸三铵、酒石酸、乙酸铵等有机基体改进剂对消除基体干扰效果。前二者均有效地消除基体干扰,但1％抗坏血酸 1％柠檬酸三铵混合试剂的效果更好,它不仅可以消除基体干扰,还可降低背景及噪声,Cr的吸收峰也较平滑。本法准确,相对偏差在0.7—4.4％范围内。回收率在92—109％范围内。若海水Cr含量低于定量下限时,可采用多次进样法。     

重油凝胶色谱制备样品中痕量镍的分析研究

研究表明微波密闭消解法对重油凝肢色谱制各样品的前处理，不造成易挥发有机金属化合物的损失，对样品无污染。采用消解前定容，配合石墨炉二次进样富集样品，可以测定样品中低至10^—9级的镍。方法应用于镍在渣油中随相对分子质量分布分析中，标准样品对照数据吻合好，相对标准偏差(RSD，n＝11)为8％。     

涂钨热解石墨管－石墨炉原子吸收法测定天然水中痕量钡

选择涂钨热解石墨管测钡，克服了钡的碳化物形成而提高了方法的灵敏度，采用钙做基体补偿不仅克服钙对测钡的影响，同时也对测钡起增敏作用，结合其它测定条件的优化实现了石墨炉原子吸收法测定天然水中的痕量钡。其线性范围在０～７０μｇ／Ｌ检出限３．３ｐｇ，特征质量为２．９ｐｇ／１％吸收，对５μｇ／ＬＢａ试液测定１１次，其ＲＳＤ为６．９％，加标回收率８９％～１２０％。方法经标样分析验证，结果与标准值相符。     

石墨炉原子吸收分光光度法测定土壤样品中痕量镉

研究了土壤样品中痕量镉的石墨炉原子吸收分光光度法测定最佳条件以及磷酸二氢铵与硝酸镁作基体改进剂对测定镉的基体改进效应，并比较了两种试样分解体系。方法检出限为0.01pg／L，精密度(RSD，n=8)为3．29％-7．69％，经国家一级标准物质分析验证，结果与标准值符合。     

石墨炉原子吸收光谱法测定土壤样品中镉

采用磷酸氢二铵作基体改进剂塞曼扣背景石墨炉原子吸收光谱法测定土壤样品中镉，方法检出限DL=0．012μg／g，精密度RSD在3．55％～7．33％，满足了土壤样品中镉测定的镉质量要求。     

石墨炉塞曼原子吸收光谱法测定硅酸盐中微量砷

本法采用氯酸钾-王水分解样品,选用硝酸镍作基体改进剂,提高了灰化温度。使用石墨杯原子化器,Zeeman效应扣除背景,实现了用石墨炉原子吸收法直接测定硅酸盐中微量砷。快速、简便,其绝对灵敏度达5.7×10~(-11)(g/l％),变动系数小于8％。     

Eolian deposition determined by the oxygen plasma furnace

The oxygen plasma furnace enables small samples of clastic sediment to be separated from filter papers at low temperatures without physical or chemical alteration of the sediment. This technique provides a suitable treatment for processing very small samples of alpine eolian sediment, enabling their grain size distribution, mineralogy, and origin to be determined.     

Sandstone response to salt weathering following simulated fire damage: a comparison of the effects of furnace heating and fire

Fire has long been recognized as an agent of rock weathering. Our understanding of the impact of fire on stone comes either from early anecdotal evidence, or from more recent laboratory simulation studies, using furnaces to simulate the effects of fire. This paper suggests that knowledge derived from simulated heating experiments is based on the pre‐conceptions of the experiment designer – when using a furnace to simulate fire, the operator decides on the maximum temperature and the duration of the experiment. These are key factors in determining the response of the stone to fire, and if these are removed from real‐world observations then knowledge based on these simulations must be questioned. To explore the differences between heating sandstone in a furnace and a real fire, sample blocks of Peakmoor Sandstone were subjected to different stress histories in combination (lime rendering and removal, furnace heating or fire, frost and salt weathering). Block response to furnace heating and fire is discussed, with emphasis placed on the non‐uniformity of the fire and of block response to fire in contrast to the uniform response to surface heating in a furnace. Subsequent response to salt weathering (by a 10% solution of sodium chloride and magnesium sulphate) was then monitored by weight loss. Blocks that had experienced fire showed a more unpredictable response to salt weathering than those that had undergone furnace heating – spalling of corners and rapid catastrophic weight loss were evidenced in blocks that had been subjected to fire, after periods of relative quiescence. An important physical side‐effect of the fire was soot accumulation, which created a waxy, relatively impermeable layer on some blocks. This layer repelled water and hindered salt ingress, but eventually detached when salt, able to enter the substrate through more permeable areas, concentrated and crystallized behind it, resulting in rapid weight loss and accelerated decay. Copyright © 2007 John Wiley & Sons, Ltd.