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Measurement uncertainty from physical sample preparation of moss samples: Estimation of mechanical cleaning vs. rinsing

机译:来自苔藓样品的物理样品制备的测量不确定度:机械清洁与漂洗的估计

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摘要

Next to sampling, the physical sample preparation step is a second large source of uncertainty. To assess the level of uncertainty from sampling, sample preparation and analysis of moss material, 27 combined and duplicate samples of moss species Pleurozium schreberi (Brid.) Mitt were collected and prepared for analysis using two different treatment methods After sampling had been done, samples were dried at an ambient temperature and then each primary and duplicate sample was divided into two sub samples for preparation. The first sub-sample was manually cleaned whereas the second one was triple rinsed with deionized water and left to dry. Subsequently, the samples were milled and digested in a close microwave system with 8 mL of HNO3 (1:1) and 1 mL of 30% H2O2. In all samples Cu, Fe and Zn were determined using GFAAS and FAAS techniques. Each sample was analyzed twice. Sampling, sample preparation and analytical uncertainty were calculated using ANOVA, RANOVA, modified RANOVA and range statistics methods. Sampling and sample preparation uncertainty varied from 3.8 to 19.8% and from 3.6 to 11.2%, respectively. For all the elements examined analytical uncertainty was below 1.1%. The comparison of element concentrations in manually cleaned and rinsed samples showed that rinsed samples were enriched in Cu and Zn, as opposed to manually cleaned that in turn displayed raised levels of Fe. However, except for Zn, these differences were not statistically significant. (C) 2017 Elsevier Ltd. All rights reserved.
机译:除了采样外,物理样品制备步骤是不确定性的第二大来源。为了评估来自采样,样品制备和苔藓材料分析的不确定性水平,收集了27种合并和重复的苔藓物种白灵菇(Brid。Mitt)的样品,并准备使用两种不同的处理方法进行分析。在环境温度下干燥,然后将每个主要和重复样品分成两个子样品进行制备。手动清洁第一个子样本,而第二个子样本用去​​离子水冲洗三次,然后晾干。随后,将样品研磨并在密闭的微波系统中用8 mL的HNO3(1:1)和1 mL的30%H2O2进行消解。在所有样品中,使用GFAAS和FAAS技术测定了Cu,Fe和Zn。每个样品分析两次。使用ANOVA,RANOVA,改进的RANOVA和范围统计方法计算采样,样品制备和分析不确定度。采样和样品制备的不确定度分别为3.8%至19.8%和3.6%至11.2%。对于所有检查的元素,分析不确定度均低于1.1%。比较手工清洗和漂洗样品中元素的浓度,可以发现漂洗样品中的铜和锌含量较高,而手工清洗后的样品中铁含量升高。但是,除锌外,这些差异在统计学上不显着。 (C)2017 Elsevier Ltd.保留所有权利。

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