Mercury determination in various environmental, food and material complex matrices using unified operating conditions for a cold vapor generation high-resolution continuum source quartz tube atomic absorption spectrometry method.

An analytical method with broad applicability based on cold vapor generation high-resolution continuum source quartz tube atomic absorption spectrometry was developed and evaluated for the determination of total mercury in matrices with various complexities and compositions. Sample preparation for different matrices of food, environmental samples and (bio)polymeric materials and unified operating conditions for derivatization and measurement were evaluated. The method was validated according to established requirements (Eurachem Guide 2014, EC Decisions 657/2002; 333/2007; 836/2011 and Association of Official Analytical Chemists Guide - AOAC). Analytical versatility was checked on various samples of fish fillets, mushrooms, soil, water and water sediment, sludge from a wastewater treatment unit, and (bio)polymeric materials from waste recycled from food packaging, computers and garden tools. Under optimal conditions for cold vapor generation in a batch system, namely 3% (v/v) HCl as reaction medium for 5 mL aliquot samples and a volume of 3.5 mL 0.3% (m/v) NaBH4 stabilized in 0.2% (m/v) NaOH as derivatization reagent, the detection limit for Hg in terms of peak height measurement (n = 7 days) was in the range 0.064 ± 0.004 µg L-1 in water, 0.014 ± 0.001 mg kg-1 in environmental samples and 0.009 ± 0.001 mg kg-1 in (bio)polymeric materials. Overall recovery of Hg by analysis of certified reference materials was 102 ± 20% (k = 2) in food, soil, wastewater and water sediment, and polyethylene. Precision for the measurement of various real samples ranged between 4.2 and 15.0%. A performance study highlighted that the method was sensitive, free of non-spectral interference coming from the multielemental matrix and that it complied with the requirements for Hg determination set in EC Decisions and AOAC Guidelines at least for the more common matrices analyzed for social impact.

Unified analysis method for total and inorganic As determination in foodstuffs by hydride generation high-resolution continuum source quartz tube atomic absorption spectrometry.

A unified analytical method applicable to common foodstuff matrices was developed and characterized for total and inorganic arsenic determination by hydride generation high-resolution continuum source quartz tube atomic absorption spectrometry, which was established based on different sample preparation procedures. This new method was found to be interference-free and cost-effective in terms of reagents consumption for sample preparation and derivatization to arsine for the inorganic arsenic fraction. Microwave-assisted digestion in HNO3-H2O2 for total arsenic and extraction in 0.28 mol L-1 HNO3 by mechanical stirring in a water bath or ultrasound-assisted extraction in 0.01 mol L-1 HCl without separation of inorganic As, all coupled with arsine generation in 0.01 mol L-1 HCl medium with 0.6% NaBH4 in 0.01% NaOH in the presence of 0.2% L-cysteine was found to be suitable for all matrices. The results were statistically compared by applying Tukey's and Dunnett's multiple comparison methods (p > 0.05). The use of external calibration with As(III) standards and standard addition method for quantification showed the lack of non-spectral interferences from the multimineral matrices, resulting in a reliable method for total/inorganic As determination in various foodstuffs. The limits of detection for total/inorganic As using peak height measurement were 0.0044 ± 0.0005/0.0022 ± 0.0003 mg kg-1 (n = 25 days). The overall recovery for total/inorganic As in the certified reference materials was in the range of 98% ± 22%, and 99% ± 24% (k = 2). The extraction of inorganic As in 0.01 mol L-1 HCl and 0.28 mol L-1 HNO3 provided the recovery of 106% ± 25% and 100% ± 25% (k = 2), which was better than in 10 mol L-1 HCl. The precision of measurements in real samples of fish muscle, meat and organs, rice and rice-based baby foods with contents of 0.052-5.29 mg kg-1 total As and 0.005-0.063 mg kg-1 inorganic As was 9.8-18.8% and 8.7-32.0%, respectively, which was calculated based on the combined uncertainty.