Coedo A G, Padilla I, Dorado M T
Centro Nacional de Investigaciones Metalúrgicas (CSIC), Avda. Gregorio del Amo, 8, 28040 Madrid, Spain.
Talanta. 2005 Jul 15;67(1):136-43. doi: 10.1016/j.talanta.2005.02.029. Epub 2005 Mar 23.
Element determination in solid waste products from the steel industry usually involves the time-consuming step of preparing a solution of the solid. Laser ablation (LA) inductively coupled plasma mass spectrometry (ICP-MS) has been applied to the analysis of Cr, Ni, Cu, As, Cd and Sn, elements of importance from the point of view of their impact on the environment, in electric arc furnace flue dust (EAFD). A simple method of sample preparation as pressed pellets using a mixture of cellulose and paraffin as binder material was applied. Calibration standards were prepared spiking multielement solution standards to a 1:1 ZnO+Fe(2)O(3) synthetic matrix. The wet powder was dried and mechanically homogenised. Quantitative analysis were based on external calibration using a set of matrix matched calibration standards with Rh as a internal standard. Results obtained using only one-point for calibration without matrix matched, needing less time for standardization and data processing, are also presented. Data are calculated for flue dust reference materials: CRM 876-1 (EAFD), AG-6203 (EAFD), AG-6201 (cupola dust) and AG-SX3705 (coke ashes), and for two representative electrical arc furnace flue dusts samples from Spanish steelmaking companies: MS-1 and MS-2. For the reference materials, an acceptable agreement with certificate values was achieved, and the results for the MS samples matched with those obtained from conventional nebulization solutions (CN). The analytical precision was found to be better than 7% R.S.D. both within a single pellet and between several pellets of the same sample for all the elements.
钢铁行业固体废物中的元素测定通常涉及制备固体溶液这一耗时步骤。激光烧蚀(LA)电感耦合等离子体质谱(ICP-MS)已应用于电弧炉烟尘(EAFD)中铬、镍、铜、砷、镉和锡的分析,从这些元素对环境的影响来看,它们都很重要。采用了一种简单的样品制备方法,即将纤维素和石蜡的混合物作为粘结剂材料压制成丸粒。校准标准物质通过向1:1的ZnO + Fe₂O₃合成基质中加入多元素溶液标准物质来制备。湿粉末经干燥并进行机械匀化。定量分析基于外标法,使用一组与基体匹配的校准标准物质,并以铑作为内标。还给出了仅使用单点校准且不进行基体匹配时获得的结果,这种方法标准化和数据处理所需时间较少。计算了烟尘标准物质的相关数据:CRM 876 - 1(电弧炉烟尘)、AG - 6203(电弧炉烟尘)、AG - 6201(冲天炉粉尘)和AG - SX3705(焦炭灰),以及来自西班牙钢铁公司的两个代表性电弧炉烟尘样品:MS - 1和MS - 2的数据。对于标准物质,获得了与证书值可接受的一致性,并且MS样品的结果与从传统雾化溶液(CN)获得的结果相匹配。发现所有元素在单个丸粒内以及同一样品的几个丸粒之间的分析精密度均优于7%相对标准偏差。