1. Method development and production of an ambient-stable blood certified reference material for total mercury, methylmercury, and trace elementsKoichi Haraguchi, Mineshi Sakamoto, Hiromitsu Nagasaka, Milena Horvat, Ermira Begu, Polona Klemenčič, Adna Alilović Osolin, Masaaki Nakamura, 2026, original scientific article Abstract: Background. Certified reference materials (CRMs) for mercury speciation of biological fluids have hitherto been limited to frozen or cold-storage types, which impedes the participation of laboratories in tropical or remote regions. Existing CRMs often do not fully meet user needs, particularly regarding storage stability and concentration relevance. Results. Using pooled Japanese human blood, we developed a freeze-dried, ambient-stable blood CRM, with certified values of 6.16 μg L−1 for total mercury (THg) and 5.46 μg L−1 for methylmercury (MeHg, as Hg). These concentrations are congruent with median exposure levels in fish-consuming populations (e.g., small island states and riverine Amazonian communities) derived from global biomonitoring data. Homogeneity, stability, and traceability were validated through inter-laboratory comparisons and rigorous uncertainty assessment. Significance. This ambient-stable blood CRM broadens global access to high-quality QA/QC of mercury speciation, especially in regions lacking cold-chain infrastructure. It contributes to capacity building under the Minamata Convention and strengthens interlaboratory comparability. Registration in COMAR and international collaborative deployment are under active development, enhancing the global infrastructure for mercury biomonitoring.
Keywords: passive monitoring, methylmercury, blood samples, mercury detection, human biomonitoring, trace elements
Published in DiRROS: 04.05.2026; Views: 143; Downloads: 108
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2. Sustainable mercury monitoring using graphitic carbon nitride as a 2D binding layer in diffusive gradient thin filmsDmitrii Deev, Raghuraj S. Chouhan, Igor Živković, Ermira Begu, Ana Drinčić, Francisco Ruiz-Zepeda, Andraž Krajnc, Ivan Jerman, Roman Viter, Aleš Lapanje, Milena Horvat, 2026, original scientific article Abstract: Mercury (Hg) is a highly toxic and persistent environmental pollutant whose accurate monitoring remains challenging due to limitations in existing diffusive gradients in thin films (DGT) binding materials, including insufficient selectivity, complex synthesis, and sustainability concerns. In this study, we report the first application of graphitic carbon nitride (GCN) nanosheets as a metal-free and sustainable binding material for Hg²⁺ monitoring in DGT systems, addressing key limitations of current approaches. Few-layer GCN nanosheets were synthesized via thermal polymerization followed by protonation-assisted exfoliation and comprehensively characterized using X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), transmission electron microscopy (TEM), atomic force microscopy (AFM), Raman spectroscopy, and scanning electron microscopy (SEM). These analyses confirmed the formation of a structurally stable, nitrogen-rich framework with abundant coordination sites. The GCN–agarose (AG–GCN) composite binding layer demonstrated high mercury binding efficiency (>90%) at environmentally relevant concentrations (2.5–10 ng/mL) and near-neutral pH, attributed to strong coordination between Hg²⁺ ions and electron-donating nitrogen sites within the heptazine structure. Compared to conventional DGT binding phases, the proposed system offers enhanced sustainability, metal-free composition, and strong affinity toward mercury, highlighting its potential for next-generation passive environmental monitoring and advanced nanomaterial-based sensing platforms.
Keywords: passive monitoring, graphitic carbon nitride nanosheets, adsorbent, mercury detection, nanosheets
Published in DiRROS: 04.05.2026; Views: 164; Downloads: 109
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3. Human hair certified reference material for total mercury, methylmercury, and trace element analysesAkane Yamakawa, Kimiyo Nagano, Kaoru Onishi, Miyuki Ukachi, Milena Horvat, Adna Alilović Osolin, Polona Klemenčič, Ermira Begu, Marta Jagodic Hudobivnik, Keisuke Uchida, 2025, original scientific article Abstract: The National Institute for Environmental Studies (NIES) developed the NIES CRM No. 13-a, a new certified reference material for human hair, using scalp hair from Asian females. This CRM represents a significant advancement in support of global mercury exposure assessments and offers unparalleled reliability and scope compared with existing materials. We aimed to provide a comprehensive overview of the preparation, certification, and application of NIES CRM No. 13-a. In total, 806 bottles (3 g each) were produced, with thorough homogenization ensured through sieving and blending. Certified values for total mercury (1.06 ± 0.07 mg/kg), methylmercury (0.858 ± 0.075 mg/kg), and key trace elements (arsenic, cadmium, lead, selenium, and zinc) were determined through extensive collaborative analyses involving 20 laboratories. Additional reference values were provided for calcium, magnesium, sodium, sulfur, antimony, barium, copper, iron, and manganese. Rigorous stability and homogeneity assessments demonstrated the stability of the CRM for over 10 years and consistency across sample units, even for challenging elements such as selenium. The CRM also includes information values of stable mercury isotope ratios, reflecting their growing importance as exposure tracers. This enhancement in accuracy and traceability facilitates accurate mercury and trace element assessments in human hair, enabling improved biomonitoring of mercury exposure, dietary studies, toxicological evaluations, human health risk evaluations, and regulatory compliance.
Keywords: metilirano živo srebro, methylmercury, certified reference material
Published in DiRROS: 05.09.2025; Views: 663; Downloads: 309
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4. Achieving measurement comparability in mercury speciation analysis in seawater : Key requirements and best practicesIgor Živković, Lars-Eric Heimbürger-Boavida, Mariia V. Petrova, Aurélie Dufour, Ermira Begu, Milena Horvat, 2025, original scientific article Abstract: The comparability of measurement results is an important issue in contemporary mercury (Hg) speciation in seawater. Sampling campaigns must be properly designed to determine significant differences on spatial and temporal scales, considering two major parameters: the variability of expected data at a given sampling point/ transect and variability in the results due to the intrinsic properties of specific analytical methods, particularly the measurement uncertainty. This study assessed the required sample size, considering several aspects of data variability when determining total Hg, dissolved gaseous Hg, and methylated Hg species in seawater. The required sample sizes were calculated using (1) the measurement uncertainty of a single-laboratory measurement of analytical methods used; (2) performance of the laboratories in interlaboratory comparison exercises; and (3) natural variability in Hg species/fractions in a selected case study in the Central Adriatic Sea. It was shown that the measurement uncertainty of a particular method and interlaboratory variability among laboratories have significant influence on data interpretation in case natural variability of Hg fractions is relatively small, such as for example the open seawater depth profiles. In contrary, in areas with large natural variability of Hg con tractions, such as coastal and contaminated sites, their influence on data interpretation is negligible. The present paper introduces the importance of proper estimation of measurement uncertainty in international programs, such as GEOTRACES, where data comparability is of fundamental importance to assess temporal and spatial trends of Hg measurements in the marine environment
Published in DiRROS: 05.09.2025; Views: 635; Downloads: 178
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