A solid-spiking matrix matched calibration strategy for simultaneous determination of cadmium and chromium in sediments by isotope dilution laser ablation inductively coupled plasma mass spectrometry,Journal of Analytical Atomic Spectrometry

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A solid-spiking matrix matched calibration strategy for simultaneous determination of cadmium and chromium in sediments by isotope dilution laser ablation inductively coupled plasma mass spectrometry
Journal of Analytical Atomic Spectrometry ( IF 3.1 ) Pub Date : 2020/01/28 , DOI: 10.1039/c9ja00335e
J. Terán-Baamonde _{1,

2,

3,

4,

5} , A. Carlosena _{1,

2,

3,

4,

5} , R. M. Soto-Ferreiro _{1,

2,

3,

4,

5} , J. M. Andrade _{1,

2,

3,

4,

5} , A. Cantarero-Roldán _{4,

5,

6,

7,

8} , S. Muniategui-Lorenzo _{1,

2,

3,

4,

5}

Affiliation

A rapid solid-spiking matrix-matched strategy is applied to simultaneously determine Cd and Cr in sediments by laser ablation inductively coupled plasma isotope dilution mass spectrometry (LA-ICP-IDMS). For this, conventional instrumentation (i.e. nanosecond laser device and ablation chamber) frequently available in laboratories is used. Two drying procedures for the synthesis of the isotopically enriched solid spike were studied considering precision, as RSD values, and applying nested ANOVA statistics; where from it was found that rotary evaporation mixed the spike solution with the solid matrix best. Thus, the solid spike is prepared using a drying step which reduced significantly the time of the synthesis, from hours (reported in literature) to minutes. The elemental distribution of the target isotopes in the pellets was assessed for natural isotope composition materials, solid spikes and enriched blend samples, and it was statistically demonstrated that the ablation of only five lines per pellet provided satisfactory precision. The time of the measurement step of the mass spectrometer was reduced compared to conventional instrumental conditions, programming a unique sequence to measure Cd (in low mass resolution) and Cr (in medium mass resolution) in the same ablation line. The study of the variables affecting the ablation process by means of a Plackett–Burman experimental design revealed that the method was robust. Accuracy was studied, both trueness (experimental/certified values ratios around unity) and precision (relative standard deviations around 2% and 4% for Cd, and 7% and 10% for Cr, when analyzing SRM 1944 and PACS-3, respectively), with good results. Satisfactory relative uncertainties in the range 10–17% were obtained. The important task of the applicability of the proposed approach (not often found in the literature) was demonstrated by the analysis of marine sediments collected at the Northwest coast of Spain.

中文翻译：

固体加标基质匹配的校准策略，通过同位素稀释激光烧蚀电感耦合等离子体质谱法同时测定沉积物中的镉和铬

采用快速固相混合基质匹配策略，通过激光烧蚀-电感耦合等离子体同位素稀释质谱法（LA-ICP-IDMS）同时测定沉积物中的镉和铬。为此，常规仪器（即使用实验室经常使用的纳秒激光装置和消融室。研究了两种干燥方法，用于合成同位素富集的固体峰，考虑了精度（作为RSD值）并应用了嵌套ANOVA统计数据；从中发现旋转蒸发将加标溶液与固体基质混合得最好。因此，使用干燥步骤制备固体掺料，该干燥步骤将合成时间从数小时（文献报道）显着减少至数分钟。对于天然同位素组成材料，固体尖峰和富集的混合样品，评估了颗粒中靶同位素的元素分布，并且统计证明每个颗粒仅消融5条线即可提供令人满意的精度。与传统仪器条件相比，质谱仪的测量步骤时间缩短了，编程了一个独特的序列以在同一条消融线上测量Cd（低质量分辨率）和Cr（中质量分辨率）。通过Plackett-Burman实验设计对影响消融过程的变量进行的研究表明，该方法是可靠的。在分别分析SRM 1944和PACS-3时，研究了准确性（真实性（实验值/认证值比率约为1）和精度（镉的相对标准偏差分别为2％和4％，铬为7％和10％））。，效果很好。相对不确定度在10％至17％之间。

更新日期：2020-03-12

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