Cold Vapor Atomic Fluorescence Spectrometry Research Articles

DEVELOPMENT AND VALIDATION OF A METHOD FOR THE DETERMINATION OF MERCURY IN SMALL RAT BRAIN TISSUE SAMPLES BY COLD VAPOR ATOMIC FLUORESCENCE SPECTROMETRY

ABSTRACT A rugged, sensitive, semi-automated method for the determination of trace-level mercury in small rat brain tissue samples by cold vapor atomic fluorescence spectrometry (CVAFS) is described. Small tissue aliquots (100 mg) are digested for 6–8 h at an elevated temperature in a mixture of nitric and sulfuric acids. Following digestion, samples are oxidized with potassium bromate/bromide at room temperature and treated with a continuous flow of stannous chloride to generate mercury vapor. The experimentally determined method quantitation limit (MQL) in the rat brain matrix is 10 pg Hg/mL, which corresponds to 1.5 ng Hg/g brain tissue. Replicate matrix spike preparations (n = 4) at this level were determined with a high level of accuracy (89.8%) and precision (6.9% RSD). Replicates (n = 36) of a certified reference material (DOLT-2, trace metals in dogfish liver) were prepared and analyzed over a four year period in order to assess the ruggedness and accuracy of the method. The average recovery for mercury in this material was 99.9% of the certified level.

Direct determination of methylmercury and inorganic mercury in biological materials by solid sampling-electrothermal vaporization-inductively coupled plasma-isotope dilution-mass spectrometry.

This paper reports on the use of solid sampling-electrothermal vaporization-inductively coupled plasma mass spectrometry (SS-EIV-ICPMS) for the direct and simultaneous determination of methylmercury and inorganic mercury in biological materials. The main advantage of this fast and sensitive method is that no sample preparation is required. In this way, the sample throughput can be considerably increased, problems of contamination and analyte losses are kept to a minimum and, even more important, the original chemical form of the different analyte species in the solid samples is preserved. To achieve this goal, a solid sample is inserted into a graphite furnace of the boat-in-tube type and is subsequently submitted to an appropriate temperature program, leading to the separate vaporization of methylmercury and inorganic mercury, which are transported into the ICP by means of an argon carrier gas. The separation was accomplished within 75 s. For the quantification of the two peaks, species-unspecific isotope dilution was used. For this purpose, a stable flow of argon loaded with gaseous Hg isotopically enriched in 200Hg was generated using a permeation tube that was constructed in-house. Its emission rate was determined by collecting the mercury released during a given time interval on a gold-coated silica absorber, after which the amount collected was released by heating of the absorber and determined by cold vapor atomic absorption spectrometry (CVAAS) and cold vapor atomic fluorescence spectrometry (CVAFS). A reference material from the Canadian National Research Council (NRC) (TORT-2) was used to assess the accuracy of the method. For the application of the method to samples with diverse mercury contents, the spike/sample ratio can be optimized by varying the emission rate of the permeation tube simply by adapting its temperature. To prove the feasibility of this approach, two reference materials (BCR 463 and DORM-2) with a methylmercury content more than 10 times higher than that of TORT-2 were also analyzed. The detection limits obtained for 1 mg of sample (2 ng g(-1) and 6 ng g(-1) for methylmercury and inorganic mercury, respectively) were found to be sufficiently low for this kind of application and are competitive when compared to other techniques.

Determination of methylmercury in human hair by ethylation followed by headspace solid-phase microextraction–gas chromatography–cold-vapour atomic fluorescence spectrometry

An analytical procedure for the determination of methylmercury in human hair after acid digestion using aqueous ethylation, headspace solid-phase microextraction sampling and final gas chromatography–cold-vapour atomic fluorescence spectrometry detection is described. Acid digestion, extraction procedure and chromatographic conditions were optimised. An optimal linear range using standard mercury solutions was found and concentration detection limits for the mercury species, MeHg and Hg 2+, were about 50 and 80 ng/g, respectively, for 100 mg of human hair. The reproducibility of the developed analytical procedure assessed for hair samples with incurred MeHg was better than 18% ( n=5). A certified reference material from the National Institute of Environmental Studies (Japan) was used for validation. Analysis of human hair collected from urban inhabitants was performed and the mean value of methylmercury content in hair samples was 0.764±0.732 μg/g for the population tested. The developed analytical method is simple, fast and a suitable procedure for the monitoring and screening of human exposure to methylmercury.

Determination of mercury by continuous flow cold vapor atomic fluorescence spectrometry using micromolar concentration of sodium tetrahydroborate as reductant solution.

Systematic experiments were conducted to evaluate and compare the analytical figures of merit of two reducing agents (SnCl2 and NaBH4) in a continuous flow cold vapor atomic fluorescence mercury analyzer. It was found that sodium tetrahydroborate can efficiently reduce Hg2+ in various environmental samples at a concentration as low as 10 microM (ca. 3.8 x 10(-5)% w/v). Most commonly encountered transition metals (Fe2+, Fe3+, Zn2+, Cu2+, Ni2+, Pb2+ and Cr3+) did not interfere with total Hg determination. No interference from hydride-forming elements (Se4+, Sb3+ and As3+) was observed. Interference caused by Mn2+ and Ag+ could be readily removed by dilution and by using appropriate modification of the reaction matrix. A higher concentration of NaBH4 (0.1 M) is stable for I month when stored in the NaOH matrix (0.2 M) and at low temperature (4 degrees C). A working solution of NaBH4 can be freshly prepared by dilution. With NaBH4, the whole continuous flow system is kept clean much more easily as no precipitate is formed, which in turn considerably reduces memory effects, simplifies analytical operation and reduces the chemical cost six-fold.

Cold vapour atomic fluorescence spectrometry and gas chromatography-pyrolysis-atomic fluorescence spectrometry for routine determination of total and organometallic mercury in food samples.

Two procedures have been investigated for the quantification of the different forms of mercury in food. A two-stage procedure has been developed to determine firstly total inorganic and organometallic species, and then the full separation of all organomercury species. The procedure involves solubilisation of the samples using alkaline extractions or enzymolysis, followed by the extraction of organic mercury in an organic solvent, preferably a mixture of dichloromethane and hexane (3:2). For the total organic mercury determination, the organic extract is analysed for "total" mercury after nitric acid/peroxide digestion, evaporation of the solvent and detection by cold vapour-atomic fluorescence spectrometry. Full organomercury speciation requires a clean-up step before analysis of the final extract in dichloromethane by gas chromatography coupled to a pyrolyser and an atomic fluorescence detector (GC-pyro-AFS). A detection limit of 6 ng l-1, and reproducibility of 2% was achieved for the CV-AFS method; GC-pyro-AFS yielded 200 ng l-1 and 5% for detection limit and coefficient of variation, respectively. Both procedures were validated with the use of various certified reference materials over a wide range of mercury concentrations, and by spiking experiments. The validated methods were tested successfully on a wide range of commercially available food samples.

Simple methodology for methylmercury and inorganic mercury determinations by high-performance liquid chromatography–cold vapour atomic fluorescence spectrometry

An analytical methodology was developed to separate and quantify methylmercury (MeHg) and inorganic mercury by high-performance liquid chromatography (HPLC)–cold vapour atomic fluorescence spectrometry (CV-AFS). The use of UV oxidation of the organic forms of mercury, the tin(II) chloride reduction in acidic medium of mercury and the introduction of a water vapour trap based on H 2SO 4/CaCl 2 resulted in a low detection limit (DL) (10±2 pg, mean value±S.D.). The apparatus was operationally optimised through the modified simplex method leading to an increase of the signal by a factor of 2. The method performance has been tested by determining the MeHg concentration in a sediment certified reference material (CRM) and the results were statistically indistinguishable from the certificate value ( α=0.05) both for the mean value and S.D.

EXAMINATION OF DIETARY METHYLMERCURY EXPOSURE IN THE CASA PIA STUDY OF THE HEALTH EFFECTS OF DENTAL AMALGAMS IN CHILDREN

This study examined methylmercury concentrations in blood of children participating in the Casa Pia Study of the Health Effects of Dental Amalgams in Children over a 1-yr period and related them to their diets in terms of fish and other seafood consumption. One hundred and fifty children between the ages of 8 and 10 yr who were residents of the Casa Pia School System of Lisbon, Portugal, participated. Parents or caregivers completed a food frequency questionnaire designed specifically for this study at baseline. Children provided urinary and blood samples for mercury determinations at baseline and at 1 yr following placement of dental tooth fillings. Mercury levels in fish samples from children's diets were also obtained. Mercury determinations in urine, blood, and fish were performed using cold vapor atomic fluorescence spectroscopy. The mean value of baseline methylmercury concentrations in blood increased as the report of seafood consumption increased, although not statistically significantly. However, blood methylmercury and total mercury concentrations were significantly lower at 1-yr follow-up than at baseline. Sixty-one percent of parents/caregivers reported that their children consumed fish on a weekly basis. The fish offered at a sample of the schools contained low levels of methylmercury (range 13.9-23.6 ng/g). Thus, children participating in the Casa Pia dental amalgam study are exposed to low dietary levels of methylmercury by way of fish consumption, and this finding was reflected in the low mean blood methylmercury concentrations observed. The present findings indicate that dietary methylmercury is not a significant source of mercury exposure and is not likely to confound the association of dental amalgam mercury with potential health effects in the present study.

Determination of very low levels of dissolved mercury(II) and methylmercury in river waters by continuous flow with on-line UV decomposition and cold-vapor atomic fluorescence spectrometry after pre-concentration on a silica gel-2-mercaptobenzimidazol sorbent

A new, simple and sensitive method for the simultaneous determination of mercury(II) and methylmercury chloride at sub-ng l −1 levels in river waters is described. Inorganic and organic mercury were preconcentrated from fresh water samples simultaneously on a laboratory-made column containing 2-mercaptobenzimidazol loaded on silica gel and then quantitatively eluted with 0.05 M KCN solution and 2.0 M HCl to desorp inorganic and methylmercury species, respectively. After irradiation with an intensive UV source, MeHg + was decomposed and mercury vapours were generated from inorganic and organic mercury using an acidic SnCl 2 solution in a continuous flow system and were subsequently determined with a cold vapour atomic fluorescence (CV-AFS) spectrometer. Detection limits (3 σ) were 0.07 and 0.05 ng l −1 (as Hg) for mercury(II) chloride and methylmercury chloride, respectively. Relative standard deviations of method (%R.S.D.) were 8.8 and 10 for inorganic and organomercuric species in the river water, respectively. The analysis of real samples, taken from different rivers, showed that inorganic mercury levels ranged from 4.0±0.6 to 12±1 ng l −1 (as Hg and 95% confidence limit) and methylmercury levels at 0.2±0.02 ng l −1(as Hg).

Effects of 2,3-dimercapto-1-propanesulfonic acid (DMPS) on tissue and urine mercury levels following prolonged methylmercury exposure in rats.

Methylmercury, a potent neurotoxicant, accumulates in the brain as well as the kidney during chronic exposure. We evaluated the capacity of 2,3-dimercapto-1-propanesulfonic acid (DMPS), a tissue-permeable metal chelator, to reduce brain, kidney, and blood Hg levels and to promote Hg elimination in urine following exposure of F-344 rats to methylmercury hydroxide (MMH) (10 ppm) in drinking water for up to 9 weeks. Inorganic (Hg2+) and organic (CH3Hg+) mercury species in urine and tissues were assayed by cold vapor atomic fluorescence spectroscopy (CVAFS). Following MMH treatment for 9 weeks, Hg2+ and CH3Hg+ concentrations were 0.28 and 4.80 microg/g in the brain and 51.5 and 42.2 microg/g in the kidney, respectively. Twenty-four hours after ip administration of a single DMPS injection (100 mg/kg), kidney Hg2+ and CH3Hg+ declined 38% and 59%, whereas brain mercury levels were slightly increased, attributable entirely to the CH3Hg+ fraction. Concomitantly, Hg2+ and CH3Hg+ in urine increased by 7.2- and 28.3-fold, respectively, compared with prechelation values. A higher dose of DMPS (200 mg/kg) was no more effective than 100 mg/kg in promoting mercury excretion. In contrast, consecutive DMPS injections (100 mg/kg) given at 72-h intervals significantly decreased total mercury concentrations in kidney, brain, and blood. However, the decrease in brain and blood mercury content was restricted entirely to the CH3Hg+ fraction, consistent with the slow dealkylation rate of MMH in these tissues. Mass balance calculations showed that the total amount of mercury excreted in the urine following successive DMPS injections corresponds quantitatively to the total amount of mercury removed from the kidney, brain, and blood of MMH-exposed rats. These findings confirm the efficacy of consecutive DMPS treatments in decreasing mercury concentrations in target tissue and in reducing overall mercury body burden. They demonstrate further that the capacity of DMPS to deplete tissue Hg2+ is highly tissue-specific and reflects the relative capacity of the tissue for methylmercury dealkylation. In light of this observation, the inability of DMPS to reduce Hg2+ levels in brain or blood may explain the inefficacy of DMPS and similar chelating agents in the remediation of neurotoxicity associated with prolonged MMH exposure.

Irreversible precipitation of mercury and lead

There are immediate concerns with current commercial reagents that are used for heavy metal precipitation; in particular the fact that the reagents are not specifically designed to bind the targeted metals. The current literature reveals that not only do commercial reagents lack sufficient ability to strongly bind the metals, but they also fail to provide long-term stability as ligand–metal complexes under a variety of moderate conditions. For this reason a new ligand was designed and synthesized: 1,3-benzenediamidoethanethiol (BDETH 2). It offers multiple, concerted, bonding sites for heavy metals and forms a stable metal–ligand precipitate. In this study, the formation of compounds comprised of this ligand with the divalent metals, lead and mercury, was explored and the pH stability of the water insoluble precipitates was determined. The leaching properties of the metal–ligand precipitates were determined using inductively coupled plasma (ICP) spectroscopy and cold vapor atomic fluorescence spectroscopy (CVAF). The results indicate that a 50.00 ppm lead solution at a pH of 4.0 may be reduced to a concentration of 0.05 ppm (99.9% lead removal) and to 0.13 ppm (99.7% lead removal) at a pH 6.0. A 50.00 ppm mercury solution at pH 4.0 may be reduced to a concentration of 0.02 ppm (99.97% mercury removal) and to 0.02 ppm (99.97% mercury removal) at a pH of 6.0.

Selective determination of thiolic proteins by hydrophobic interaction chromatography coupled with on-line cold vapour atomic fluorescence spectrometry

A new analytical method is proposed for the determination and characterization of thiolic proteins, based on hydrophobic interaction chromatography (HIC) coupled on-line with cold vapour atomic fluorescence spectrometry (CVAFS). Thiolic groups are derivatized pre-column by p-hydroxymercurybenzoate (PHMB) and the derivatized proteins are separated on a TSKgel Ether-5PW column. Post-column on-line reaction of derivatized proteins with bromine, generated in situ by KBr/KBrO3 in HCl medium, allowed the fast conversion of protein-bound PHMB to inorganic mercury, Hg(II), which is selectively detected by AFS after sodium borohydride reduction to Hg0. Under optimized conditions, on-line bromine treatment gives a 85 ± 2% recovery of both free and protein-complexed PHMB in less than 2.5 s and at room temperature. Glyceraldehyde-3-phosphate dehydrogenase, aldolase, pyruvate kinase, trioso phosphate isomerase and phospho-glucose isomerase have been examined. Sensitivity and limit of detection of proteins depends on the number of –SH groups reacting with PHMB and are in the range of 10−8–10−9 mol dm−3 with calibration curves spanning over four decades of concentration.

Distribution of inorganic mercury in Sacramento River water and suspended colloidal sediment material.

The concentration and distribution of inorganic Hg was measured using cold-vapor atomic fluorescence spectrometry in samples collected at selected sites on the Sacramento River from below Shasta Dam to Freeport, CA, at six separate times between 1996 and 1997. Dissolved (ultrafiltered, 0.005 microm equivalent pore size) Hg concentrations remained relatively constant throughout the system, ranging from the detection limit (< 0.4 ng/L) to 2.4 ng/L. Total Hg (dissolved plus colloidal suspended sediment) concentrations ranged from the detection limit at the site below Shasta Dam in September 1996 to 81 ng/L at the Colusa site in January 1997, demonstrating that colloidal sediment plays an important role in the downriver Hg transport. Sequential extractions of colloid concentrates indicate that the greatest amount of Hg associated with sediment was found in the "residual" (mineral) phase with a significant quantity also occurring in the "oxidizable" phase. Only a minor amount of Hg was observed in the "reducible" phase. Dissolved Hg loads remained constant or increased slightly in the downstream direction through the study area, whereas the total inorganic Hg load increased significantly downstream especially in the reach of the river between Bend Bridge and Colusa. Analysis of temporal variations showed that Hg loading was positively correlated to discharge.

On-site mercury analysis of soil at hazardous waste sites: by immunoassay and ASV

Two field methods for Hg, immunoassay and anodic stripping voltammetry (ASV), that can provide onsite results for quick decisions at hazardous waste sites were evaluated. Each method was applied to samples from two Superfund sites that contain high levels of Hg; Sulphur Bank Mercury Mine site, Clear Lake, California, and Carson River Mercury site, Nevada. Two laboratory methods were used for comparison purposes; cold vapor atomic fluorescence spectrometry (CVAFS) and inductively coupled plasma-mass spectrometry (ICP-MS). The immunoassay was found to be accurate for high and low Hg concentrations compared to the 5 and 15 μg/g soil sample standards provided with it. Despite poor agreement between immunoassay and confirmatory analysis results at concentrations near the comparison standards, the immunoassay could be used as an effective screening method provided care is taken in identifying an operational screening level. The ASV method had an analytical range of 1–50 μg/g, with a CV of 15%. ASV results were comparable to CVAFS (CV=15%) and more precise than ICP-MS (CV=20%). The lower limit of quantitative results was 3 μg/g for field samples, and is attributed to uncertainty associated with sampling.

Longitudinal Study of Methylmercury and Inorganic Mercury in Blood and Urine of Pregnant and Lactating Women, as Well as in Umbilical Cord Blood

We have investigated exposure to methylmercury (MeHg) and mercury vapor (Hg0) in pregnant women and their newborns in Stockholm. The women were followed for 15 months post delivery. MeHg, inorganic Hg (I-Hg), and total Hg (T-Hg) in maternal and cord blood were determined by automated alkaline solubilization/reduction and cold vapor atomic fluorescence spectrometry. T-Hg in urine was determined by inductively coupled plasma mass spectrometry. About 72% of the Hg in blood (n=148) in early pregnancy was MeHg (median 0.94 μg/L, maximum 6.8 μg/L). Blood MeHg decreased during pregnancy, partly due to decreased intake of fish in accordance with recommendations to not eat certain predatory fish during pregnancy. Cord blood MeHg (median 1.4 μg/L, maximum 4.8 μg/L) was almost twice that in maternal blood in late pregnancy and was probably influenced by maternal MeHg exposure earlier and before pregnancy. Blood I-Hg (median 0.37 μg/L, maximum 4.2 μg/L) and urine T-Hg (median 1.6 μg/L, maximum 12 μg/L) in early pregnancy were highly correlated, and both were associated with the number of amalgam fillings. The concentrations decreased during lactation, probably due to excretion in milk. Cord blood I-Hg was correlated with that in maternal blood. The results show the importance of speciation of Hg in blood for evaluation of exposure and health risks.

Development of a method for the determination of ultra-trace level mercury in adipose tissue by cold vapour atomic fluorescence spectrometry

Development of a method for the determination of ultra-trace level mercury in adipose tissue by cold vapour atomic fluorescence spectrometry

A methodological study of mercury speciation using dogfish liver CRM (DOLT-2).

The purpose of the study was to optimise analytical methods for determination of the chemical speciation of mercury in studies of protective mechanisms of selenium. Optimisation of the methods was performed using CRM DOLT-2 (Dogfish liver), both in its original form and after separation of various fractions. The sample was homogenised with 10 mM Tris-HCl buffer (pH 7.6) and ultracentrifuged. The soluble phase obtained was applied to a size exclusion chromatography column (Sephadex G-75 column) for separation of various protein fractions. Total mercury (total Hg), monomethyl mercury (MeHg) and selenium (Se) were determined in whole dogfish liver tissue and its soluble and insoluble phases (pellet). Different approaches for determination of total Hg and MeHg were compared. Simultaneous determination of MeHg and inorganic mercury (Hg2+) was based on alkaline dissolution and/or acid leaching, followed by ethylation, room temperature precollection, isothermal gas chromatography (GC), pyrolysis and detection with cold vapour atomic fluorescence spectrometry (CVAFS). The sum of MeHg and Hg2+ was compared to total Hg results obtained by acid digestion and CVAAS detection. The accuracy of MeHg determination was checked by its determination using acid leaching at room temperature, solvent extraction, back extraction into Milli-Q water, ethylation, GC and CVAFS detection. For the insoluble phase it is recommended to use solvent extraction for MeHg and acid digestion CVAAS for total Hg. For determination of MeHg and Hg2+ in the lyophilised sample and water soluble fractions containing low concentrations of mercury species, the simultaneous measurement of MeHg and Hg2+ after alkaline dissolution is the most appropriate method.

Improved determination of gaseous divalent mercury in ambient air using KCl coated denuders.

An improved method for the determination of gaseous divalent mercury (GDM) in ambient air using KCl coated denuders has been developed and tested. GDM collected in the KCl coated denuders can be quantitatively desorbed at 450 degrees C in 10 min. After being complete thermally reduced to Hg0 at 900 degrees C, all mercury released from the denuder is pre-concentrated on the analytical Au trap, and detected by cold vapor atomic fluorescence spectrometry (CVAFS). The absolute detection limit of the method is less than 3 pg. Preliminary data of GDM concentration in ambient air from different sampling stations show that GDM concentrations in the urban air of Göteborg are much higher than in rural air (Rörvik and Sasetta), which indicates the anthropogenic origin of GDM.

Analysis and stability of mercury speciation in petroleum hydrocarbons.

Raw petroleum and natural gas often contain high concentrations of mercury, which can be damaging to the metal components of production facilities, as well as to the environment. Various Hg species have different properties in terms of mobility, reactivity and bioavailability. Thus, for cost-effective decisions regarding plant design, Hg extraction, and pollution control, speciation information must be available at the production facility. In this paper, a simple, wet chemical speciation method, which provides data on Hg(o), dissolved and particulate total Hg, Hg(II), and methyl Hg is presented. The method incorporates species-specific extraction and separation procedures, followed by cold vapor atomic fluorescence spectrometry (CVAFS). For each species, detection limits of approximately 0.1 ng/g were obtained. Storage experiments in various containers showed that organo-mercury species were stable for at least 30 days in all containers except those made of polyethylene; and Hg(o) was stable in all containers except those made of stainless steel or polyethylene. Hg(II) was rapidly lost from all containers except those made of aluminum, which rapidly converted it to Hg(o), which was stable. In general, most of the total Hg in petroleum products was particulate Hg, followed by dissolved Hg(II) and Hg(o). Sub-ng/g concentrations of methyl-Hg were observed in most samples.

Development of a method for the determination of ultra‐trace level mercury in adipose tissue by cold vapour atomic fluorescence spectrometry

A method for the determination of total mercury in rat adipose tissue by cold vapour atomic fluorescence spectrometry (CVAFS) has been developed. Adipose samples were initially subjected to a lyophilization procedure in order to facilitate the homogenization and accurate weighing of small tissue aliquots (~50 mg). A closed vessel microwave digestion procedure using a mixture of sulphuric and nitric acids was used to liberate mercury from the adipose matrix. All mercury species were quantitatively oxidized to Hg(II) by a potassium bromate/bromide oxidation, then reduced to Hg(0) vapour by stannous chloride prior to fluorescence detection. The CVAFS exhibited a linear range of 10 pg Hg/ml to 120 pg Hg/ml. The method detection limit in solution was 2 pg Hg/ml, or 1 ng Hg/g adipose tissue, based on a nominal 50 mg sample and a final volume of 25 ml. A reference material from the National Research Council of Canada (DOLT-2, trace metals in dogfish liver) was prepared in quadruplicate in order to assess the accuracy and precision of the method. Mercury in this material was recovered at 2.22 ± 0.08 μ g/g, which is 104% of the certified level (2.14 ± 0.10 μ g/g).

Microwave-assisted determination of total mercury and methylmercury in sediment and porewater

Existing methods for total mercury and methylmercury determination in sediment and porewaters were improved by applying open microwave heating for extraction of Hg species from the sample and decomposition of MeHg prior to detection as Hg(II) by CV AFS. It was shown that nitric acid can quantitatively leach Hg from sediment, already at a low microwave power (30 W, 5 min). Methylmercury can be quantitatively leached from sediment by dilute sulphuric acid (1 mol/L) at a power of 60 W during 5 minutes, without being decomposed. So obtained extract can be further distilled with a reduced possibility for artefac- tual MeHg formation, as it contains much lower levels of inorganic Hg, compared to the original sediment. Microwave-assisted BrCl oxidation was shown to be more effective for decomposition of MeHg and stable organomercury complexes in water solu- tions (sediment distillate and porewater), as compared with BrCl oxidation at room-temperature. Therefore, the application of low-power microwave digestion can significantly improve determination of Hg species in sediment and porewater, both in terms of time and efficiency.