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首页> 外文期刊>Fuel >Trace element analysis of gasification plant samples by i.c.p.--m.s.: validation by comparison of results from two laboratories
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Trace element analysis of gasification plant samples by i.c.p.--m.s.: validation by comparison of results from two laboratories

机译：i.c.p .-- m.s。对气化厂样品的痕量元素分析：通过比较两个实验室的结果进行验证

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In the absence of either standard methods for trace element analysis of coal-derived chars and ash or standard reference materials for coal gasification samples, a comparative exercise has been undertaken to validate analyses of chars and fines recovered from a coal gasification Pilot plant. Several sample digestion methods, used for converting solid samples to aqueous solutions for trace element analysis by i.c.p.--m.s. and i.c.p.--a.e.s., have been compared: peroxide fusion (sodium peroxide + sodium carbonate) and microwave digestion by AEA Technology and wet-ashing (open acid digestion) and microwave digestion by Imperial College (IC). The aim was to analyse samples from a pilot plant scale coal gasification rig. Digestions were carried out using a range of sample sizes, at times as small as l0 mg and analyses of small quantities of these samples were compared with results on the same samples from a specialist contract laboratory (AEA Technology). Elements studied were As, B, Ba, Be, Cd, Co, Cr, Cu, Ga, Hg, Mn, Mo, Ni, Pb, Sb, Se, Sn, V and Zn. For the majority of the elements studied, elemental concentrations (l--l50 wppm range) were generally in agreement between the two laboratories within 50/100. Limitations of the various digestion methods are discussed. All the digestion techniques appeared to lose mercury and therefore a Leco atomic absorption spectrophotometer based method was used to determine Hg. Output solid stream distributions of trace elements from the gasifier indicate that all of the Hg in the fuels was released to the fuel gas. The primary cyclone fines stream contained the major part of the trace elements from the fuels. The causes of apparent losses of As, Mo, Pb, Sn, Zn and Se are discussed.
机译：在既没有标准方法来分析源自煤的焦炭和灰分的痕量元素，也没有针对煤气化样品的标准参考材料的情况下，已经进行了比较实验以验证从煤气化中试厂回收的焦炭和细粉的分析。几种样品消解方法，用于通过i.c.p .-- m.s。将固体样品转化为水溶液进行痕量元素分析。比较了i.c.p.和a.e.s .：过氧化物融合（过氧化钠+碳酸钠）和AEA技术进行微波消解，湿灰化（开放式酸消解）和帝国理工学院（IC）进行微波消解。目的是分析中试规模的煤气化装置的样品。使用一定范围的样品进行消化，有时小至10 mg，并将少量样品的分析结果与来自专业合同实验室（AEA Technology）的相同样品的结果进行比较。研究的元素为As，B，Ba，Be，Cd，Co，Cr，Cu，Ga，Hg，Mn，Mo，Ni，Pb，Sb，Se，Sn，V和Zn。对于所研究的大多数元素，两个实验室之间的元素浓度（l-1wwppm范围）通常在50/100之内。讨论了各种消化方法的局限性。所有的消化技术似乎都损失了汞，因此使用了基于Leco原子吸收分光光度计的方法来测定Hg。气化炉中微量元素的输出固体流分布表明，燃料中的所有汞都释放到了燃料气体中。初级旋风细粉流包含燃料中痕量元素的大部分。讨论了As，Mo，Pb，Sn，Zn和Se的表观损耗的原因。

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