A reliable method to prepare milligram size environmental samples to quantify metal(loid)s by high-resolution graphite furnace atomic absorption spectrometry

IF 1.6 Q2 MULTIDISCIPLINARY SCIENCES

MethodsX Pub Date : 2024-08-08 DOI:10.1016/j.mex.2024.102896

Patrícia Gomes Costa, Juliana Lemos Dal Pizzol, Yuri Dornelles Zebral, Adalto Bianchini

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Abstract

We searched for an extraction method that would allow a precise quantification of metal(loid)s in milligram-size samples using high-resolution graphite furnace atomic absorption spectrometry (HR-GFAAS). We digested biological (DORM-4, DOLT-5 and TORT-3) and sediment (MESS-4) certified reference materials (CRMs) using nitric acid in a drying oven, aqua regia in a drying oven, or nitric acid in a microwave. In addition, we digested MESS-4 using a mixture of nitric and hydrofluoric acids in a drying oven. We also evaluated the effect of sample size (100 and 200 mg) on the extraction efficiency. Nitric acid extraction in a drying oven yielded the greatest recovery rates for all metal(loid)s in all tested CRMs (80.0 %–100.0 %) compared with the other extraction methods tested (67.3 %–99.2 %). In most cases, the sample size did not have a significant effect on the extraction efficiency. Therefore, we conclude that nitric acid digestion in a drying oven is a reliable extraction method for milligram-size samples to quantify metal(loid)s with HR-GFAAS. This validated method could provide substantial benefits to environmental quality monitoring programs by significantly reducing the time and costs required for sample collection, storage, transport and preparation, as well as the amount of hazardous chemicals used during sample extraction and analysis.

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Sample digestion with nitric acid in a drying oven yielded the greatest recovery rates of metal(loid)s from biological and sediment certified reference materials.
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The recovery rates of metal(loid)s from biological and sediment certified reference materials using nitric acid digestion in a drying oven ranged from 73 % to 100 %.
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Digestion with nitric acid in a drying oven is a simple and reliable method to extract small size environmental samples for metal(loid)s quantification by high-resolution graphite furnace atomic absorption spectrometry.

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制备毫克级环境样品的可靠方法，可通过高分辨率石墨炉原子吸收光谱法量化金属（惰性）物质

我们一直在寻找一种提取方法，以便利用高分辨率石墨炉原子吸收光谱（HR-GFAAS）对毫克级样品中的金属（loid）进行精确定量。我们使用干燥箱中的硝酸、干燥箱中的王水或微波炉中的硝酸消化了生物（DORM-4、DOLT-5 和 TORT-3）和沉积物（MESS-4）的标准物质（CRM）。此外，我们还在干燥箱中使用硝酸和氢氟酸的混合物消化了 MESS-4。我们还评估了样品量（100 毫克和 200 毫克）对提取效率的影响。与其他测试的萃取方法（67.3%-99.2%）相比，在干燥箱中进行硝酸萃取对所有测试的 CRM 中的所有金属（loid）的回收率最高（80.0%-100.0%）。在大多数情况下，样品量对萃取效率没有显著影响。因此，我们认为在干燥箱中进行硝酸消解是一种可靠的萃取方法，可用于毫克级样品的 HR-GFAAS 定量。这种经过验证的方法可以大大减少样品采集、储存、运输和制备所需的时间和成本，以及样品提取和分析过程中使用的危险化学品的数量，从而为环境质量监测项目带来巨大的效益。-在干燥箱中用硝酸消解是一种简单可靠的方法，可提取小粒径环境样品，用高分辨率石墨炉原子吸收光谱法进行金属（loid）定量分析。

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