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Analysis of polyacrylamide gels for trace metals using diffusive gradients in thin films and laser ablation inductively coupled plasma mass spectrometry

机译:使用薄膜中的扩散梯度和激光烧蚀电感耦合等离子体质谱法分析痕量金属的聚丙烯酰胺凝胶

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A simple method for the analysis of polyacrylamide diffusive gradients in thin film (DGT) gels by laser ablation inductively coupled plasma mass spectrometry (LA-ICPMS), employing a novel use of In-115 internal standardization, has been developed. This method allows the determination of Co, Ni, Cu, Zn, Cd, and Pb concentrations (at the DGT filter face) or fluxes in sediments at a spatial resolution of 100 mum. Single-layered gels, using an optimized laser defocus of 4000 mum at 400 mJ power, showed high precision (generally similar to10%) and a linear response during solution deployment. Of the elements Sc, In, Ba, La, Ce, and Tb, Ba most closely tracked variations in laser energy and showed the highest analytical precision but could not be used as an internal standard due to its elevated presence in natural sediments. Therefore, internal standardization, necessary to normalize data collected on different days, was carried out using In-115 contained within a second layer of backing gel and dried along with the analyte layer as a dual-gel disk. This multilayered gel standard required a laser defocus setting of 1000 mum and a laser power of similar to800 mJ. Analytical precision for a 64-spot ablation grid at 100-mum spacing similar to10%. Verification of this method was carried out on DGT sediment probes deployed in Priest Pot (English Lake District). Results obtained by conventional slicing techniques and aqueous elution agreed with laser ablation results when the different sampling areas were considered. The elution results varied by a factor of < 2, whereas the laser ablation technique showed a variability of similar to4, indicating localized elevated concentrations of Co. This higher resolution LA-ICPMS method could ultimately lead to an improved understanding of the geochemical processes responsible for metal uptake and release in sediments.
机译:已经开发了一种简单的方法,该方法利用In-115内部标准化技术的新颖用途,通过激光烧蚀感应耦合等离子体质谱(LA-ICPMS)分析薄膜(DGT)凝胶中的聚丙烯酰胺扩散梯度。这种方法可以确定Co,Ni,Cu,Zn,Cd和Pb浓度(在DGT过滤器表面)或沉积物中通量的空间分辨率为100微米。单层凝胶在400 mJ功率下使用4000 mm的最佳激光散焦,显示出高精度(通常接近10%)和溶液部署过程中的线性响应。在元素Sc,In,Ba,La,Ce和Tb中,Ba最能追踪激光能量的变化并显示出最高的分析精度,但由于其在天然沉积物中的含量较高,因此不能用作内标。因此,使用包含在第二层衬里凝胶中的In-115进行内部标准化,这是标准化在不同日期收集的数据所必需的,并与分析物层一起干燥作为双凝胶盘。这种多层凝胶标准品要求将激光散焦设置为1000 mm,激光功率应接近800 mJ。 64点消融栅格在100毫米间距处的分析精度接近10%。该方法的验证是在Priest Pot(英国湖区)部署的DGT沉积物探针上进行的。当考虑不同的采样面积时,通过常规切片技术和水洗脱获得的结果与激光消融结果相符。洗脱结果的变化因数小于2,而激光烧蚀技术显示的变异性近似于4,表明局部浓度的Co升高。这种更高分辨率的LA-ICPMS方法可能最终导致人们对导致地球化学过程的认识有所改善金属吸收并在沉积物中释放。

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