Speciation of Mercury in Environmental Water Samples with Seasonal Change

2011 ◽  
Vol 264-265 ◽  
pp. 1690-1695
Author(s):  
M.M. Rahman ◽  
Alias Mohd Yusof

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.

Author(s):  
Ha Le Van ◽  
Minh Hien Lu Thi ◽  
Chau Nguyen Minh ◽  
Giang Tran Hoang ◽  
Hien Dang Thi ◽  
...  

In this study, iodide and iodate species in food were simultaneously determined by LC-ICP-MS after sample treatment with Deion water based on ultrasonic extraction. The conditions of the instrument and the extraction procedure were investigated. The method was validated with calibration curves that have the coefficient of determination (R2) higher than 0.995. The method limits of detection (LOD) of iodide and iodate were 0.079 and 0.060 mg/kg respectively meeting the regulatory requirements for food safety management. The recoveries were in the range of 83.5 - 108% and the relative standard deviations (RSDr) were between 2.57 and 5.22%. These parameters met the requirements specified by AOAC. A total of 43 salty spice samples including table salts, iodized seasoning soup powders, seasoning seeds, oyster sauces, soy sauces, fish sauces were collected and analyzed for research purposes. The results showed that a high percentage (76.9%) of table salt and seasoning soup powder samples had total iodate and iodide content lower than the specified level. Meanwhile, other salty spice samples, especially seasoning seeds and soy sauces, had a significant content of iodide in the range of 2.0 to 13.2 mg/kg. This study has contributed to the preliminary assessment of the current status of iodine content in salty spice products collected in Hanoi city.


2012 ◽  
Vol 10 (4) ◽  
pp. 1175-1182 ◽  
Author(s):  
Elisaveta Mladenova ◽  
Ivanka Dakova ◽  
Dimiter Tsalev ◽  
Irina Karadjova

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.


2019 ◽  
Vol 85 (4) ◽  
pp. 110-113
Author(s):  
Olexandr Ponomarenko ◽  
Anatolyi Samchuk ◽  
Kateryna Vovk ◽  
Igor Shvaika ◽  
Ganna Grodzinskaya

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.


2007 ◽  
Vol 90 (3) ◽  
pp. 844-856 ◽  
Author(s):  
Kaare Julshamn ◽  
Amund Maage ◽  
Hilde Skaar Norli ◽  
Karl H Grobecker ◽  
Lars Jorhem ◽  
...  

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.


2010 ◽  
Vol 93 (1) ◽  
pp. 323-326 ◽  
Author(s):  
Ni Zhang ◽  
Zhiying Ding ◽  
Hao Li ◽  
Xin Wang ◽  
Xiaodong Shao

Abstract A practical and nontarnishing method for the determination of trace nickel (Ni) in hydrogenated cottonseed oil by inductively coupled plasma/mass spectrometry (ICP/MS) was developed. In order to avoid tarnishing in the pretreatment of samples, the technology of pressurized PTFE vessel acid digestion was applied. The temperature and acid content in the digestion were optimized. The results showed that hydrogenated cottonseed oil could be digested completely by the proposed method. Compared with the U.S. Pharmacopeia 28 and British Pharmacopoeia 2003 methods, the developed method avoided the risk of using platinum and the tarnish from silica crucibles. In addition, the analytical cycle of the test solution was shortened by the use of ICP/MS instead of graphite furnace atomic absorption spectrophotometry.


1994 ◽  
Vol 77 (5) ◽  
pp. 1299-1304 ◽  
Author(s):  
Paul H Shtonen ◽  
Harold C Thompson

Abstract A method was developed to analyze various calcium supplements for Ca and Pb content. The analysis involves a dry ash of the supplements followed by wet digestion. The Pb is determined by graphite furnace atomic absorption spectro–photometry (GFAAS). Analysis of Ca is by inductively coupled plasma–atomic emission spectrometry (ICP–AES). Ca supplements fortified with Pb at levels ranging from 0.25 to 10.0 μg/g yielded recoveries ranging from 82.7 ± 4.2 to 105.0 ± 1.7%. To test accuracy, the method was applied to National Institute of Standards and Technology standard reference materials (NIST SRMs) 1572 citrus leaves and 1486 bone meal. GFAAS analysis of SRM 1572 averaged 13.1 ± 0.6 μg Pb per g (certificate value, 13.3 ± 2.4 (μg Pb per g), and analysis of SRM 1486 averaged 1.34 ± 0.11 μg Pb per g (certificate value, 1.335 ± 0.014 μg Pb per g). ICP–AES analysis of SRM 1572 averaged 3.12 ± 0.01% Ca (certificate value, 3.15 ± 0.10% Ca by weight), and analysis of SRM 1486 averaged 27.63 ± 0.27% Ca (certificate value, 26.58 ± 0.24% Ca). The method's limit of quantitation (LOQ), on supplement Ca basis and a 1 g sample, averaged 0.75 μg Pb per 1 g Ca for supplements containing 9 to 35% Ca by weight. At a Pb level of 0.663 μg/g Ca, the reproducibility relative standard deviation (RSDr) averaged 7.3% and the repeatability relative standard deviation (RSDr) averaged 8.0%. It is recommended that the method be studied collaboratively.


2011 ◽  
Vol 264-265 ◽  
pp. 1684-1689 ◽  
Author(s):  
M.M. Rahman ◽  
Alias Mohd Yusof ◽  
A.K.H. Wood ◽  
A. Shamsiah

A simple and less expensive solvent extraction method was used with inductively coupled plasma mass spectrometry (ICP-MS) in the speciation of two environmentally significant, toxic forms of arsenic: arsenite and arsenate. Dissolved inorganic arsenic species in drinking waters from reservoirs and treatment plants were determined by the inductively coupled plasma mass spectrometry analyses. Prior to the analysis the water samples were precocentrated by solvent extraction using APCDT to separate the arsenic species from elemental interferences. The detection limit of this method achieved was 0.059 gL-1. The suitability of the technique in this work is discussed in relation to risk assessment studies of public health.


2021 ◽  
Vol 245 ◽  
pp. 03004
Author(s):  
Yanxia Zeng ◽  
Xiashi Zhu

A subject for the rapid determination of iodine content in drinking water by isopropyl sensitization and ICP-MS was established. The samples were dissolved in 1% ammonia solution, 127I was selected as the mass number to be measured and 159Tb as an internal standard. At the same time, 4% (V/V) isopropanol was used to enhance aerosol gasification efficiency, 2% NH3·H2O was used to effectively eliminate memory effects of iodine by cleaning sample for 180 seconds. The results show that, the detection limits of iodine in this method are 0.007 mg·kg-1 and it is superior to other literature. The standard curve has a good linear relationship and the recovery rates of testing rusults range are from 96.00% to 112.3%. The content of iodine in standard substance water samples was determined by ICP-MS method. The iodine content in water samples from seven drinking water sources in Lianyungang area was analyzed between 14~21 μg·L-1. It was in line with the allowable value of 10~300 μg·L-1 of the sanitary standard for drinking water, suggesting that the iodine content of drinking water resources in Lianyungang area was in a safe range.


1984 ◽  
Vol 67 (2) ◽  
pp. 277-280
Author(s):  
Dipankar Chakraborti ◽  
Kurt J Irgolic ◽  
F Adams

Abstract Arsenite—but not arsenate, methylarsonic acid, or dimethylarsinic acid—is extracted from water samples by 5 mL of a 0.01M hexane solution of rec-dibutylthiophosphate. A 10 μL aliquot of the extract is injected into an atomic absorption spectrometer with a graphic furnace for the determination of arsenic. The calibration curve is linear to 1500 Dg As. Quantities of arsenic as low as 100 ng As (0.2 ppb As when contained in 500 mL) can be confidently determined. The method was tested with natural river water and synthetic river water. The relative standard deviations associated with the recoveries of arsenite from natural water and synthetic river water spiked with arsenite range from 4.8 to 8.0%. Ten to 15 arsenite determinations can be completed in 1h.


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