Assignation of inorganic mercury and methylmercury mass fractions in a soil matrix certified reference material by two analytical methodologies based on species‐specific isotope dilution mass spectrometry and chromatographic separation

Abstract

Assignment of inorganic mercury and methyl mercury mass fractions at an ultratrace level in soil certified reference material EnvCRM 03 with a complex matrix composition was undertaken. Inorganic mercury and methyl mercury contents by species-specific isotope dilution inductively coupled plasma mass spectrometry with on-line high-performance liquid chromatography or with classical off-line chromatography were established. Different extraction protocols: sequential extraction ((1) H 2 SO 4 /KBr/CuSO 4 ; (2) dichloromethane; (3) Na 2 S 2 O 3 ) or one-step extraction (diluted HCl) in solid-liquid systems were verified. Sequential extraction allowed quantification and separation of inorganic mercury and methyl mercury on HPLC column in one chromatographic run and were found to be (316 ± 10) μg/kg (U = 3.2%, k = 2) and (0.53 ± 0.02) μg/kg (U = 3.8%, k = 2), respectively. Extraction by diluted HCl and application of classical off-line chromatography led to the separation of methyl mercury from predominant inorganic mercury form and was found to be (0.54 ± 0.03) μg/kg (U = 5.4%, k = 2). To the best-obtained literature knowledge, there was no available soil material aimed for speciation analysis of inorganic mercury and methyl mercury so far. Both developed analytical methodologies were found to be equally sensitive and could be successfully applied for mercury species determination in samples with the complex matrix.

Multiple approaches to characterize and visualize the chemical composition of Sijunzi Decoction comprehensively

“…It has the advantages of a fast and wide linear range, so it was used for the determination of macroelements. In contrast, ICP‐MS is equipped with an MS detector to detect ions [24]. Its excellent sensitivity and efficient capability of analysis simultaneous were considered to be a great advantage in detecting the analytes that were nanograms per liter (ng/L) or parts per trillion.…”

Atomic spectrometry update – a review of advances in environmental analysis

“…The mass fractions of 48 analytes, including the REEs and the technology-critical elements Be, Bi, Ga, Ge, Li, Nb, Sb, Ta and Tl, were determined 108 in seven plant CRMs by ICP-MS/MS to provide benchmark values for future studies . Krata 109 reported the first information on Hg speciation in a soil CRM, EnvCRM 03 from the National Metrology Institute of Turkey. Values determined by SSID-HPLC-ICP-MS were 316 ± 10 μg kg −1 for inorganic Hg and 0.54 ± 0.03 μg kg −1 for MeHg.…”

Atomic spectrometry update: review of advances in elemental speciation

“…The certification of the iHg and MeHg mass fractions in a soil certified reference material, EnvCRM 03, has been reported on. 22 Both Hg species were quantified by ss-ID-ICP-MS with either on-line HPLC or off-line AEC. The HPLC separations were undertaken using a C18 column with a mobile phase of 0.05% (v/v) 2-mercaptoethanol, 0.4% (w/v) l -cysteine, 0.5% (w/v) ammonium acetate, and 2% (v/v) methanol flowing at 1 mL min −1 for 8 minutes.…”

“…The first of these is covered in Section 2 as it concerns the certification of a soil CRM. 22 The second paper describes the procedures used to distinguish between deposited and in situ formed MeHg in soils in a Swiss valley. 86 Two separate procedures, iHg spiking and double-spike (isotopically enriched iHg and MeHg) ID-HPLC-ICP-MS were used to determine and correct for artificial Hg methylation in a MeHg-selective acid-leaching/organic solvent extraction procedure (6 mol L −1 HCl, DCM, l -cysteine).…”