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Trace elements in coal derived liquids: analysis by ICP-MS and Mossbauer spectroscopy

机译：煤制液体中的痕量元素：ICP-MS和莫斯鲍尔光谱仪进行分析

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Concentrations of trace elements in coal derived liquids have been investigated by inductively coupled plasma-mass spectrometry (ICP- MS) and by Mossbauer spectroscopy. Liquefaction extracts prepared from the Argonne Premium Coals and a coal tar pitch have been examined. Microwave digestion in concentrated nitric acid has been shown as a suitable method for determining trace element concentrations in coal derived liquids by ICP-MS--for sample sizes as small as 3--20 mg. High concentrations of Fe were found for all extract samples (<265--l474 ppm). Ti, Cr, Mn, Co, Ga, Sb, Cs and Ba were measurable. Concentration distributions of trace elements found in the extracts bore little relation to the corresponding distributions in the original coals. The proportions of individual trace elements present in the original coals and found in the extracts, varied widely. Mossbauer spectroscopy of the extracts indicated that the high Fe-concentrations corresponded to the presence of organometallic-Fe compounds--and not to pyritic iron. There is evidence suggesting the presence of material derived from iron-storage proteins such as ferritin, but final proof is lacking. Our data suggest that other metallic ions detected in these coal derived liquids may be present in association with the organic material. Concentrations of paramagnetic metal species were found to be of the same order of magnitude as ESR spin-densities already found in coal liquids. Both types of paramagnetic species are suspected of causing loss of signal in solid state 13~C NMR.
机译：已经通过电感耦合等离子体质谱法（ICP-MS）和Mossbauer光谱法研究了煤衍生液体中痕量元素的浓度。考察了从Argonne Premium Coals和煤焦油沥青制备的液化提取物。浓硝酸中的微波消解已被证明是通过ICP-MS测定煤衍生液体中微量元素浓度的合适方法-样品量小至3--20 mg。所有提取物样品中都发现高浓度的铁（<265--4744 ppm）。可测量Ti，Cr，Mn，Co，Ga，Sb，Cs和Ba。提取物中发现的微量元素的浓度分布与原始煤中的相应分布关系不大。存在于原始煤中和提取物中的各种微量元素的比例差异很大。提取物的Mossbauer光谱表明，高Fe含量对应于有机金属Fe化合物的存在，而不是黄铁矿。有证据表明存在源自铁存储蛋白的物质，例如铁蛋白，但缺乏最终证据。我们的数据表明，在这些煤衍生的液体中检测到的其他金属离子可能与有机物质结合存在。发现顺磁性金属物质的浓度与煤液中已经发现的ESR自旋密度的数量级相同。怀疑这两种顺磁性物质都在固态13 C NMR中引起信号损失。

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