Mercury determination and speciation analysis in surface waters

AbstractA sorbent L-cysteine grafted silica gel has been evaluated for separation and enrichment of dissolved inorganic i-Hg(II) and methylmercury CH3Hg(I) from surface waters at sub-µg L−1 concentrations. Chemical parameters for mercury species enrichment and separation have been optimized. Analytical schemes for the determination of Hg species, using selective column solid phase extraction (SPE) with continuous flow chemical vapor generation atomic absorption spectrometry (CF-CVG-AAS) or inductively coupled plasma-mass spectrometry (ICP-MS) were developed. Possibilities for on-site SPE enrichment were demonstrated as well. The limits of quantification were 1.5 and 5 ng L−1 for dissolved i-Hg(II) and CH3Hg(I) by CF-CVG-AAS and 1 and 2.5 ng L−1 by ICP-MS with relative standard deviations between 7–12% and 7–14%, respectively. The chemically modified SPE sorbent has demonstrated high regeneration ability, chemical and mechanical stability, acceptable capacity and good enrichment factors. Results for total dissolved mercury were in reasonable agreement with those from independent analyses by direct ICP-MS determinations for river waters and for estuarine water certified reference material.

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Determination of mercury species in foodstuffs using LC-ICP-MS: the applicability and limitations of the method

Czech Journal of Food Sciences ◽

10.17221/577/2013-cjfs ◽

2014 ◽

Vol 32 (No. 3) ◽

pp. 249-259 ◽

Cited By ~ 6

Author(s):

R. Koplík ◽

I. Klimešová ◽

K. Mališová ◽

O. Mestek

Keyword(s):

Hydrochloric Acid ◽

Inductively Coupled Plasma ◽

Speciation Analysis ◽

Reversed Phase ◽

Food Samples ◽

Partial Hydrolysis ◽

Mercury Species ◽

Plant Materials ◽

Icp Ms

Reversed-phase liquid chromatography hyphenated with inductively coupled plasma mass spectrometry (LC-ICP-MS) was used for mercury speciation analysis in food samples. A short chromatographic column (Purospher® RP-8e, 75 ´ 4 mm, 3 µm) and a mobile phase containing 0.02 mol/l CH3COONH4 + 0.2% (v/v) 2-mercaptoethanol (2-ME) + 1% (v/v) CH3OH were applied. A repeated extraction of samples with hydrochloric acid/2-ME solution (1 mol/l HCl + 0.2% (v/v) 2-ME) was applied as the isolation step. The results were satisfactory for most food matrices (fish, shellfish, plant materials). Conversely, to analyse high-protein animal matrices, which contain mostly the inorganic form of mercury, a procedure including partial hydrolysis using hydrochloric acid should be used. For methylmercury and inorganic divalent mercury, the LOQ values of 0.3 and 2 ng/g, respectively, can be achieved if precautionary measures against contamination are fulfilled. The method was applied for the determination of methylmercury and inorganic divalent mercury in fish, vegetables, herbs and cereal products.

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Ti-containing mesoporous silica packed microcolumn separation/preconcentration combined with inductively coupled plasma-mass spectrometry for the determination of trace Cr, Cu, Cd and Pb in environmental samples

Journal of Analytical Atomic Spectrometry ◽

10.1039/c5ja00035a ◽

2015 ◽

Vol 30 (6) ◽

pp. 1386-1394 ◽

Cited By ~ 9

Author(s):

Chao Cui ◽

Hanyong Peng ◽

Yanan Zhang ◽

Kai Nan ◽

Man He ◽

...

Keyword(s):

Mesoporous Silica ◽

Environmental Samples ◽

Inductively Coupled Plasma ◽

Solid Phase ◽

Trace Metal Analysis ◽

Inductively Coupled ◽

Icp Ms ◽

Plasma Mass Spectrometry ◽

Microcolumn Separation

Solid phase extraction with Ti-containing mesoporous silica as adsorbent combined with ICP-MS for trace metal analysis in environmental samples.

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Ultra-sensitive speciation analysis of mercury by CE-ICP-MS together with field-amplified sample stacking injection and dispersive solid-phase extraction

Electrophoresis ◽

10.1002/elps.201500460 ◽

2015 ◽

Vol 37 (7-8) ◽

pp. 1055-1062 ◽

Cited By ~ 22

Author(s):

YiQuan Chen ◽

Xian Cheng ◽

Fan Mo ◽

LiMei Huang ◽

Zujian Wu ◽

...

Keyword(s):

Solid Phase Extraction ◽

Solid Phase ◽

Speciation Analysis ◽

Phase Extraction ◽

Dispersive Solid Phase Extraction ◽

Sample Stacking ◽

Icp Ms

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Speciation of Mercury in Environmental Water Samples with Seasonal Change

Advanced Materials Research ◽

10.4028/www.scientific.net/amr.264-265.1690 ◽

2011 ◽

Vol 264-265 ◽

pp. 1690-1695

Author(s):

M.M. Rahman ◽

Alias Mohd Yusof

Keyword(s):

Seasonal Change ◽

Water Samples ◽

Methyl Mercury ◽

Inductively Coupled Plasma ◽

Potassium Dichromate ◽

Graphite Furnace ◽

Extraction Procedure ◽

Graphite Tube ◽

Icp Ms ◽

Relative Standard

Mercury concentrations and speciation were determined in surface water samples taken from rivers in the vicinity of industrial area, in Johore Malaysia. Samples were collected from the same sites before and immediately after rainfall. The aim of this study is to assess the influence of seasonal change in river water on the concentration of mercury (Hg) species. Trace concentrations of mercury in water samples were determined by a method involving a simple and rapid procedure involving the flow-injection inductively coupled plasma mass spectrometry (FI-ICP-MS) and graphite furnace atomic absorption spectrometry (GFAAS) techniques. Mercury vapor, generated by sodium borohydride as the reductant, was stabilized by potassium dichromate (K2Cr2O7), then released by controlled heating and detected by FI-ICP-MS. Methyl mercury (II) was preconcentrated using the ammonium pyrolidindithiocarbamate (APDTC)-chloroform extraction procedure and the chloroform extract was introduced into the graphite tube. The absolute detection limits were found to be 0.204 μg L-1 and 0.273 μg L-1 for total mercury and methyl mercury respectively, with thevariability being lower than 5% relative standard deviation (RSD) at the 5 μg L-1 level. Because of the high stability of MeHg (II)-APDTC complexes, it is possible to evaporate the extract in order to obtain a crystalline powder to be dissolved with a few micro liters of chloroform enacting MeHg (II) and Hg (II) can be detected at sub-nanogram levels.

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Sequential extraction and thermal desorption of mercury from contaminated soil and tailings from Mongolia

Open Chemistry ◽

10.2478/s11532-012-0074-6 ◽

2012 ◽

Vol 10 (5) ◽

pp. 1565-1573 ◽

Cited By ~ 7

Author(s):

Pavel Coufalík ◽

Pavel Krásenský ◽

Marek Dosbaba ◽

Josef Komárek

Keyword(s):

Sequential Extraction ◽

Thermal Desorption ◽

Solid Phase ◽

Extraction Procedure ◽

Speciation Analysis ◽

Water Soluble ◽

Mercury Species ◽

Different Temperatures ◽

Acidic Conditions ◽

Desorption Method

AbstractMercury forms in contaminated environmental samples were studied by means of sequential extraction and thermal desorption from the solid phase. The sequential extraction procedure involved the following fractions: water soluble mercury, mercury extracted in acidic conditions, mercury bound to humic substances, elemental Hg and mercury bound to complexes, HgS, and residual mercury. In addition to sequential extraction, the distribution of mercury species as a function of soil particles size was studied. The thermal desorption method is based on the thermal decomposition or desorption of Hg compounds at different temperatures. The following four species were observed: Hg0, HgCl2, HgS and Hg(II) bound to humic acids. The Hg release curves from artificial soils and real samples were obtained and their applicability to the speciation analysis was considered.

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Germanium determination in environmental object by the method of mass spectrometry with inductively coupled plasma

Ukrainian Chemistry Journal ◽

10.33609/0041-6045.85.4.2019.110-113 ◽

2019 ◽

Vol 85 (4) ◽

pp. 110-113

Author(s):

Olexandr Ponomarenko ◽

Anatolyi Samchuk ◽

Kateryna Vovk ◽

Igor Shvaika ◽

Ganna Grodzinskaya

Keyword(s):

Mass Spectrometry ◽

Sample Preparation ◽

Inductively Coupled Plasma ◽

Microwave Field ◽

Antitumor Effects ◽

Inductively Coupled ◽

Ms Analysis ◽

Icp Ms ◽

Relative Standard

The analytical technologies of sample preparation of rocks and mushrooms using the microwave field for the determination of germanium by the method of mass spectrometry with inductively coupled plasma (ICP-MS analysis) have been developed. Germanium is a rare element. Germanium is homology of silicon and carbon. To date, the definition of low content of germanium in geological objects is a rather complex analytical task, which requires its concentration - extraction, co-precipitation, ion exchange. At present, the harmonious combination of the method of natural objects decomposition in the microwave field and germanium determination using ICP-MS analysis is particularly promising. Sample preparation of silicate rocks for ICP-MS determination of germanium was carried out by decomposition in a mixture of hydrofluoric, phosphate and nitric acids (5: 5: 2) in a microwave oven program at 240°C for 30 min. Sample preparation of mushrooms for ICP-MS germanium determination was carried out according to the following scheme. Initially, the dried sample was sealed in the presence of CaO, after dissolving it in a mixture of HNO3+HF+H3PO4 (6:6:1). Ge solution was extracted by Nazarenko V.A. extraction method. The developed analytical schemes have made it possible to significantly reduce the duration and labor intensity of sample preparation. The obtained solutions were analyzed using an inductively coupled plasma mass spectrometer. The developed method for determining germanium by ICP-MS analysis has been successfully tested on standard rock samples. The obtained results are in accordance with the accepted attribute, the relative standard deviation Sr ranges from 0.7-0.9. The data on the content and distribution of germanium in the Boletales fungi are obtained. They indicate wild mushrooms contain high levels of germanium, especially Boletus and Mushroom biospores. These studies are necessary because the essential properties of germanium and its compounds attract special attention of scientists today. Complementary Ge compounds which have hypotensive, bactericidal, antiviral and antitumor effects have already been synthesized.

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Determination of Arsenic, Cadmium, Mercury, and Lead by Inductively Coupled Plasma/Mass Spectrometry in Foods after Pressure Digestion: NMKL Interlaboratory Study

Journal of AOAC International ◽

10.1093/jaoac/90.3.844 ◽

2007 ◽

Vol 90 (3) ◽

pp. 844-856 ◽

Cited By ~ 83

Author(s):

Kaare Julshamn ◽

Amund Maage ◽

Hilde Skaar Norli ◽

Karl H Grobecker ◽

Lars Jorhem ◽

...

Keyword(s):

Mass Spectrometry ◽

Inductively Coupled Plasma ◽

Method Performance ◽

Inductively Coupled ◽

Icp Ms ◽

Relative Standard ◽

Limit Of Quantitation ◽

Plasma Mass Spectrometry ◽

Standard Deviations

Abstract Thirteen laboratories participated in an interlaboratory method performance (collaborative) study on a method for the determination of arsenic, cadmium, mercury, and lead by inductively coupled plasma/mass spectrometry (ICP/MS) after pressure digestion including the microwave heating technique. Prior to the study, the laboratories were able to practice on samples with defined element levels (pretrial test). The method was tested on a total of 7 foodstuffs: carrot puree, fish muscle, mushroom, graham flour, simulated diet, scampi, and mussel powder. The elemental concentrations in mg/kg dry matter (dm) ranged from 0.0621.4 for As, 0.0328.3 for Cd, 0.040.6 for Hg, and 0.012.4 for Pb. The materials used in the study were presented to the participants as blind duplicates, and the participants were asked to perform single determinations on each sample. The repeatability relative standard deviations (RSDr) for As ranged from 3.8 to 24%, for Cd from 2.6 to 6.9%, for Hg from 4.8 to 8.3%, and for Pb from 2.9 to 27%. The reproducibility relative standard deviations (RSDR) for As ranged from 9.0 to 28%, for Cd from 2.8 to 18%, for Hg from 9.9 to 24%, and for Pb from 8.0 to 50%. The HorRat values were less than 1.5 for all test samples, except for the determination of Pb in wheat flour at a level close to the limit of quantitation (0.01 mg/kg dm). The study showed that the ICP/MS method is satisfactory as a standard method for elemental determinations in foodstuffs.

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