On the Chemical Form of Mercury in Edible Fish and Marine Invertebrate Tissue

1992 ◽  
Vol 49 (5) ◽  
pp. 1010-1017 ◽  
Author(s):  
Nicolas S. Bloom

Total mercury, monomethylmercury (CH3Hg), and dimethylmercury ((CH3)2Hg) in edible muscle were examined in 229 samples, representing seven freshwater and eight saltwater fish species and several species of marine invertebrates using ultraclean techniques. Total mercury was determined by hot HNO3/H2SO4/BrClldigestion, SnCl2 reduction, purging onto gold, and analysis by cold vapor atomic fluorescence spectrometry (CVAFS). Methylmercury was determined by KOH/methanol digestion using aqueous phase ethylation, cryogenic gas chromatography, and CVAFS detection. Total mercury and CH3Hg concentrations varied from 0.011 to 2.78 μg∙g−1 (wet weight basis, as Hg) for all samples, while no sample contained detectable (CH3)2Hg (<0.001 μg∙g−1 as Hg). The observed proportion of total mercury (as CH3Hg) ranged from 69 to 132%, with a relative standard deviation for quintuplicate analysis of about 10%; nearly all of this variability can be explained by the analytical variability of total mercury and CH3Hg. Poorly homogenized samples showed greater variability, primarily because total mercury and CH3Hg were measured on separate aliquots, which vary in mercury concentration, not speciation. I conclude that for all species studied, virtually ail (>95%) of the mercury present is as CH3Hg and that past reports of substantially lower CH3Hg fractions may have been biased by analytical and homogeneity variability.

The Analyst ◽  
1999 ◽  
Vol 124 (2) ◽  
pp. 185-189 ◽  
Author(s):  
Azman Shafawi ◽  
Les Ebdon ◽  
Mike Foulkes ◽  
Peter Stockwell ◽  
Warren Corns

1994 ◽  
Vol 40 (2) ◽  
pp. 206-210 ◽  
Author(s):  
S A Winfield ◽  
N D Boyd ◽  
M J Vimy ◽  
F L Lorscheider

Abstract An ultrasensitive method for determining total mercury concentrations in biological specimens is a prerequisite for monitoring exposure to chronic low-dose levels of Hg vapor such as those from dental silver amalgam fillings. The clinical consequences of such doses are currently in question. We describe an adaptation of a two-stage gold amalgamation preconcentration step combined with cold vapor atomic fluorescence spectrometric detection for Hg. At Hg concentrations of 40 and 350 nmol/L, the within-day assay CVs were 5% and 3%, respectively; between-day assay CVs were 8% and 5%, respectively. Accuracy, as demonstrated by analytical recovery, ranged from 98% to 105%. The detection limit for the assay is 50 pmol/L, which is suitable for measuring total Hg concentrations in specimens of human urine, blood, and breast milk, and in monkey kidney cortex and feces, obtained from subjects with and without amalgam fillings.


2012 ◽  
Vol 610-613 ◽  
pp. 1991-1995
Author(s):  
Mei Sun ◽  
Gui Jiang Liu ◽  
Qiang Hua Wu ◽  
Wenqi Liu

A new method was developed for the speciation of inorganic arsenic in coal samples by liquid chromatography coupled to hydride generation atomic fluorescence spectrometry after microwave-assisted extraction. Effective extract of As(III), As(V) in coal sample was achieved by 1.0molL-1 H3PO4 and 0.1 molL-1ascorbic acid. Under the optimized conditions, the limits of detection were 0.01 ugL-1and 0.02 ugL-1for As(III), As(V). The relative standard deviation were 2.4 %, 3.3 % (c= 20.0 gL-1, n=7). The proposed method was successfully applied for the determination of speciation of inorganic arsenic in coal samples and GBW11117.


1973 ◽  
Vol 27 (5) ◽  
pp. 355-361 ◽  
Author(s):  
S. R. Goode ◽  
Akbar Montaser ◽  
S. R. Crouch

A fully automated nonflame atomic fluorescence (AF) spectrometer has been constructed to facilitate a critical study of how the atomization process is affected by varying the experimental parameters. A hot wire loop atomizer is evaluated and fully optimized for atomic fluorescence spectrometry. A laboratory minicomputer or a hardware logic control system directs the spectrometer operation, including sample delivery to the atomizer, application of electrical current to heat the atomizer, data acquisition, and mathematical analysis of the data. The relative standard deviation of the data is 4 to 7%. Under most conditions on-line data processing allows variation and optimization of the parameters in real time. The optimum parameters for a platinum loop AF spectrometer are presented along with typical analytical data.


2020 ◽  
Vol 3 (2) ◽  
pp. 45
Author(s):  
Gabriela S. Yánez-Jácome ◽  
David Romero-Estévez ◽  
Hugo Navarrete ◽  
Karina Simbaña-Farinango ◽  
Pamela Y Vélez-Terreros

Several microwave-assisted digestion methods were tested at the Centro de Estudios Aplicados en Química laboratory in Quito, Ecuador, to determine the accuracy and performance efficiency of the mineralization process for the determination of total mercury in fish tissue by cold vapor atomic fluorescence spectrophotometry. The use of MARSEasyPrep high-pressure vessels, low amounts of reagents (1 cm3 HNO3, 1 cm3 H2O2, and 1 cm3 HClO4), an irradiation temperature of 210 °C, and 35 min of mineralization time resulted in accurate performance, with recoveries of certified reference material DORM-4 between 90.1% and 105.8%. This is better than the Association of Official Analytical Chemists 2015.01 method, which has a reported accuracy of 81%. The repeatability precision and intermediate precision were established at three concentration levels (0.167, 0.500, and 0.833 mg·kg−1) and expressed as the percentage of the relative standard deviation ranging from 1.5% to 3.0% and 1.7% to 4.2%, respectively. Further, the method was satisfactorily applied to analyze fortified samples of tilapia (Oreochromis niloticus), with recoveries ranging from 98.3% to 104.3%. The instrumental limits of detection and quantification were 0.118 µg·dm−3 and 0.394 µg·dm−3, respectively.


2005 ◽  
Vol 88 (2) ◽  
pp. 665-669 ◽  
Author(s):  
Jian-Bo Shi ◽  
Li-Na Liang ◽  
Gui-Bin Jiang

Abstract A comprehensive method for simultaneous determination of methylmercury (MeHg) and ethylmercury (EtHg) in rice by capillary gas chromatography (GC) coupled on-line with atomic fluorescence spectrometry was developed. The experimental conditions, including the pyrolyzer temperature and flow rates of the make-up gas and sheath gas, were optimized in detail. The absolute detection limits (3σ) were 0.005 ng as Hg for both MeHg and EtHg. The relative standard deviation values (n = 5) for 10 ng Hg/mL of MeHg and EtHg were 2.5 and 1.3%, respectively. The method was evaluated by analyzing 2 certified reference materials (DORM-2 and GBW08508), and the determined values of MeHg and total mercury concentrations were in good agreement with the certified values. In addition, the recoveries of MeHg and EtHg spiked into a rice sample collected from Jiangsu province in China were 86 and 77%, respectively. The proposed method was applied to analysis of MeHg and EtHg in 25 rice samples cultivated in 15 provinces of China. In all samples, MeHg was detectable and no EtHg was found. The MeHg contents in rice samples ranged from 1.9 to 10.5 ng/g, accounting for 7–44% of the total mercury measured.


2012 ◽  
Vol 554-556 ◽  
pp. 1669-1672
Author(s):  
Qing Shan Pan ◽  
Wei Liu ◽  
Ping Yi ◽  
Du Shu Huang ◽  
Na Wu ◽  
...  

A hydride atomic fluorescence spectrometry method was developed for the determination of trace mercury in Chinese herbal medicines. A digestion system using HNO3-H2O2 under high pressure was applied for the pretreatment of the samples. The operating condition of the instrument were optimized. The effect of the acid in sample solution and carrier liquid, and the effect of reducing agent KBH4 in solution to the determination of mercury were studied. Under the optimum conditions. Five kinds of Chinese herbal medicines in Yun Nan province of China was measured. There was a good linear coefficient between the fluorescent intensity and mercury concentration in the range of 0~10μg•L-1with a correlation coefficient of 0.9998,while the determination limits was 3.7ng•L-1,the relative standard deviation was 2.4%. The content of total mercury in the samples was 5.25~16.32ng•g-1 and a recovery range of 83.6%~109.2% were obtained.


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