Devos W, Senn-Luder M, Moor C, Salter C
Swiss Federal Laboratories for Materials Testing and Research (EMPA), Dübendorf, Switzerland.
Fresenius J Anal Chem. 2000 Apr;366(8):873-80. doi: 10.1007/s002160051588.
The suitability of laser ablation ICP-MS for minor and trace analysis of archaeological iron finds, produced by a direct reduction process in a 'bloomery' furnace, is reported. The analysis of elemental impurities in the iron can provide useful archaeometallurgical information on the production process and the provenance of the iron. Since, even after refinement, the iron resulting from this process may contain many inclusions (slag, charcoal, holes, etc.), a method should be used with sufficient spatial resolution to preclude the inclusions from the analysis. The ablation parameters are selected such that ablation craters of approx. 100 microm in diameter are obtained. The method is validated with low alloy steel and cast iron standard reference materials and by a comparative analysis with electron probe microanalysis (EPMA). The precision is limited mainly by the homogeneity of the iron, rather than by instrumental reproducibility. The advantages and drawbacks of the method are briefly compared with EPMA. Preliminary results from the analysis of archaeological iron samples from excavations at Develier-Courtetelle (Canton Jura, CH), Neftenbach (Canton Zurich, CH), Wartau (Canton St Gallen, CH) and Mont Chemin (Canton Valais, CH) are given.
本文报道了激光烧蚀电感耦合等离子体质谱法(laser ablation ICP-MS)用于分析在“鼓风炉”中通过直接还原工艺生产的考古铁制品中的微量和痕量元素的适用性。对铁中元素杂质的分析可为铁的生产工艺和来源提供有用的考古冶金信息。由于即使经过精炼,这种工艺生产的铁仍可能含有许多夹杂物(炉渣、木炭、孔洞等),因此应使用具有足够空间分辨率的方法,以避免夹杂物对分析的影响。选择烧蚀参数,使得获得直径约为100微米的烧蚀坑。该方法通过低合金钢和铸铁标准参考物质进行了验证,并与电子探针微分析(EPMA)进行了对比分析。精度主要受铁的均匀性限制,而非仪器的重现性。简要比较了该方法与EPMA的优缺点。给出了对来自瑞士汝拉州德维利耶 - 库尔泰勒、苏黎世州内夫滕巴赫、圣加仑州瓦尔陶以及瓦莱州蒙特谢曼等地考古发掘的铁样品的初步分析结果。