Chavagnac V, Milton J A, Green D R H, Breuer J, Bruguier O, Jacob D E, Jong T, Kamenov G D, Le Huray J, Liu Y, Palmer M R, Pourtalès S, Roduhskin I, Soldati A, Trueman C N, Yuan H
National Oceanography Centre Southampton, University of Southampton, European Way, Southampton SO14 3ZH, UK.
Anal Chim Acta. 2007 Sep 19;599(2):177-90. doi: 10.1016/j.aca.2007.08.015. Epub 2007 Aug 15.
Ten international laboratories participated in an inter-laboratory comparison of a fossil bone composite with the objective of producing a matrix and structure-matched reference material for studies of the bio-mineralization of ancient fossil bone. We report the major and trace element compositions of the fossil bone composite, using in-situ method as well as various wet chemical digestion techniques. For major element concentrations, the intra-laboratory analytical precision (%RSD(r)) ranges from 7 to 18%, with higher percentages for Ti and K. The %RSD(r) are smaller than the inter-laboratory analytical precision (%RSD(R); <15-30%). Trace element concentrations vary by approximately 5 orders of magnitude (0.1 mg kg(-1) for Th to 10,000 mg kg(-1) for Ba). The intra-laboratory analytical precision %RSD(r) varies between 8 and 45%. The reproducibility values (%RSD(R)) range from 13 to <50%, although extreme value >100% was found for the high field strength elements (Hf, Th, Zr, Nb). The rare earth element (REE) concentrations, which vary over 3 orders of magnitude, have %RSD(r) and %RSD(R) values at 8-15% and 20-32%, respectively. However, the REE patterns (which are very important for paleo-environmental, taphonomic and paleo-oceanographic analyses) are much more consistent. These data suggest that the complex and unpredictable nature of the mineralogical and chemical composition of fossil bone makes it difficult to set-up and calibrate analytical instruments using conventional standards, and may result in non-spectral matrix effects. We propose an analytical protocol that can be employed in future inter-laboratory studies to produce a certified fossil bone geochemical standard.
十个国际实验室参与了一项化石骨复合材料的实验室间比对，目的是制备一种基质和结构匹配的参考材料，用于古代化石骨生物矿化的研究。我们报告了该化石骨复合材料的主量和微量元素组成，采用了原位方法以及各种湿化学消解技术。对于主量元素浓度，实验室内分析精密度（%RSD(r)）范围为7%至18%，Ti和K的百分比更高。%RSD(r)小于实验室间分析精密度（%RSD(R)；<15 - 30%）。微量元素浓度变化约5个数量级（钍为0.1 mg kg⁻¹至钡为10,000 mg kg⁻¹）。实验室内分析精密度%RSD(r)在8%至45%之间变化。再现性值（%RSD(R)）范围为13%至<50%，尽管对于高场强元素（铪、钍、锆、铌）发现了极端值>100%。稀土元素（REE）浓度变化超过3个数量级，其%RSD(r)和%RSD(R)值分别为8 - 15%和20 - 32%。然而，REE模式（对于古环境、埋藏学和古海洋学分析非常重要）更加一致。这些数据表明，化石骨矿物学和化学成分的复杂且不可预测的性质使得使用传统标准设置和校准分析仪器变得困难，并可能导致非光谱基质效应。我们提出了一种分析方案，可用于未来的实验室间研究，以制备经过认证的化石骨地球化学标准物质。
