Atomic absorption spectrometry mercury determination

MDHS 14 General method for the gravimetric determination of respirable and total dust MDHS 15 Carbon disulphide MDHS 16 Mercury vapour in air Laboratory method using hopcalite adsorbent tubes, and acid dissolution with cold vapour atomic absorption spectrometric analysis MDHS 17 Benzene in air Laboratory method using charcoal adsorbent tubes, solvent desorption and gas chromatography MDHS 18 Tetra alkyl lead compounds in air Continuous on-site monitoring method using PAC Check atomic absorption spectrometry... 

Mercury was determined after suitable digestion by the cold vapour atomic absorption method [40]. Lead was determined after digestion by a stable isotope dilution technique [41-43]. Copper, lead, cadmium, nickel, and cobalt were determined by differential pulse polarography following concentration by Chelex 100 ion-exchange resin [44,45], and also by the Freon TF extraction technique [46]. Manganese was determined by flameless atomic absorption spectrometry (FAA). 

In contrast, the coupling of electrochemical and spectroscopic techniques, e.g., electrodeposition of a metal followed by detection by atomic absorption spectrometry, has received limited attention. Wire filaments, graphite rods, pyrolytic graphite tubes, and hanging drop mercury electrodes have been tested [383-394] for electrochemical preconcentration of the analyte to be determined by atomic absorption spectroscopy. However, these ex situ preconcentration methods are often characterised by unavoidable irreproducibility, contaminations arising from handling of the support, and detection limits unsuitable for lead detection at sub-ppb levels. 

Fitzgerald et al. [477] have described a method based on cold-trap preconcentration prior to gas-phase atomic absorption spectrometry for the determination of mercury down to 2 ng/1 in seawater. 

Armannsson [659] has described a procedure involving dithizone extraction and flame atomic absorption spectrometry for the determination of cadmium, zinc, lead, copper, nickel, cobalt, and silver in seawater. In this procedure 500 ml of seawater taken in a plastic container is exposed to a 1000 W mercury arc lamp for 5-15 h to break down metal organic complexes. The solution is adjusted to pH 8, and 10 ml of 0.2% dithizone in chloroform added. The 10 ml of chloroform is run off and after adjustment to pH 9.5 the aqueous phase is extracted with a further 10 ml of dithizone. The combined extracts are washed with 50 ml of dilute ammonia. To the organic phases is added 50 ml of 0.2 M-hydrochloric acid. The phases are separated and the aqueous portion washed with 5 ml of chloroform. The aqueous portion is evaporated to dryness and the residue dissolved in 5 ml of 2 M hydrochloric acid (solution A). Perchloric acid (3 ml) is added to the organic portion, evaporated to dryness, and a further 2 ml of 60% perchloric acid added to ensure that all organic matter has been... 

Batley [28] examined the techniques available for the in situ electrodeposition of lead and cadmium in estuary water. These included anodic stripping voltammetry at a glass carbon thin film electrode and the hanging drop mercury electrode in the presence of oxygen and in situ electrodeposition on mercury coated graphite tubes. Batley [28] found that in situ deposition of lead and cadmium on a mercury coated tube was the more versatile technique. The mercury film, deposited in the laboratory, is stable on the dried tubes which are used later for field electrodeposition. The deposited metals were then determined by electrothermal atomic absorption spectrometry, Hasle and Abdullah [29] used differential pulse anodic stripping voltammetry in speciation studies on dissolved copper, lead, and cadmium in coastal sea water. 

Atomic absorption spectrometry used either by direct aspiration (to determine total mercury) or as an element-specific detector for gas chromatography (to determine organically bound mercury) are now discussed. 

Millward and Bihan [59] studied the effect of humic material on the determination of mercury by flameless atomic absorption spectrometry. In both fresh and seawater, association between inorganic and organic entities takes place within 90 min at pH values of 7 or above, and the organically bound mercury was not detected by an analytical method designed for inorganic mercury. The amount of detectable mercury was related to the amount of humic material added to the solutions. However, total mercury could be measured after exposure to ultraviolet radiation under strongly acid conditions. 

Yamamoto et al. [60] determined picogram quantities of methyl mercury and total mercury in seawater by gold amalgamation and atomic absorption spectrometry. Methyl mercury was extracted with benzene and concentrated by a succession of three partitions between benzene and cysteine solution. Total mercury was extracted by wet combustion of the sample with sulfuric acid and potassium permanganate. The proportion of methyl mercury to total mercury in the coastal seawater sampled was around 1%. 

Workers at the Department of the Environment, UK [47], have described a procedure for the determination of methylmercury compounds in soils and sediments which involves extraction with a carbon tetrachloride solution of dithizone, reduction to elemental mercury then analysis by atomic absorption spectrometry. 

Li, Z., Wei, Q., Yuan, R., Zhou, X., Liu, H., Shan, H., and Song, Q., A new room temperature ionic liquid l-butyl-3-trimethylsilylimidazolium hexafluoro-phosphate as a solvent for extraction and preconcentration of mercury with determination by cold vapor atomic absorption spectrometry, Talanta, 71,68-72, 2007. 

B. Izgi, C. Demir and S. Gucer, Application of factorial design for mercury determination by trapping and graphite furnace atomic absorption spectrometry, Spectrochim. Acta, Part B, 55(7), 2000, 971-977. 

J. Moreda-Pineiro, P. Fopez-Mahia, S. Muniategui-Forenzo, E. Fernandez-Fernandez and D. Prada-Rodriguez, Direct mercury determination in aqueous slurries of environmental and biological samples by cold vapor generation-electrothermal atomic absorption spectrometry. Anal. Chim. Acta, 460(1), 2002, 111-122. 

S. Rio Segade and J. F. Tyson, Determination of methylmercury and inorganic mercury in water samples by slurry sampling cold vapor atomic absorption spectrometry in a flow injection system after preconcentration on silica C18 modified, Talanta, 71(4), 2007, 1696-1702. 

C. Schickling and J. A. C. Broekaert, Determination of mercury species in gas condensates by online coupled high-performance liquid chromatography and cold-vapor atomic absorption spectrometry, Appl. Organo-met. Chem., 9(1), 1995, 29-36. 

Carbon Monoxide. Methods for determining carbon monoxide include detection by conversion to mercury vapor, gas filter correlation spectrometry, TDLAS, and grab sampling followed by gas chromatograph (GC) analysis. The quantitative liberation of mercury vapor from mercury oxide by CO has been used to measure CO (73). The mercury vapor concentration is then measured by flameless atomic absorption spectrometry. A detection limit of 0.1 ppbv was reported for a 30-s response time. Accuracy was reported to be 3% at tropospheric mixing ratios. A commercial instrument providing similar performance is available. 

Kuwae et al. [138] have described a rapid determination of mercury in soils by high-frequency induction heating (rf) followed by cold vapour atomic absorption spectrometry. The mercury released from the sample is absorbed in stannous chloride-hydroxylamine prior to atomic absorption spectrometry. Recovery of 99.4 to 99.8% mercury was obtained by this method from portions of sample containing between 0.025-0.15 p,g of mercury. 

Cold vapour (or flameless) atomic absorption spectrometry is the method of choice for the determination of mercury in soils [136-147]. Ure and Shand [ 141 ]... 

Floyd and Sommers [142] evaluated a simple one-step digestion procedure for extracting total mercury from soils. The sample was digested with concentrated nitric acid and 4N potassium dichromate for four hours at 55 °C and the mercury in the extract determined by flameless atomic absorption spectrometry. The method can be applied to soils containing up to 20% organic matter. 

Cold vapour atomic absorption spectrometry and atomic fluorescence spectrometry (253 nm emission) have been applied to the determination of down to 0.01 mg/kg of mercury in soils and sediments [ 144],... 

Sakamoto et al. [148] have shown that the differential determinations of different forms of mercury in soil can be accomplished by successive extraction and cold vapour atomic absorption spectrometry. 

Azzaria and Aftabi [ 149] showed that stepwise (as compared to continuous) heating of soil samples before determination of mercury by atomic absorption spectrometry gives increased resolution of the different phases of mercury. A gold-coated graphite furnace atomic absorption spectrometer has been used to determine mercury in soils [150]. 

Bandyopadhyay and Das [151] extracted mercury from soils with the liquid anion exchanger Aliquat-336 prior to determination by cold vapour atomic absorption spectrometry. 

Atomic absorption spectrometry has also been used to determine mercury in multi-metal mixtures (see Sect. 2.55). 

Welz, B., D.L. Tsalev, and M. Sperling. 1992. On-line microwave sample pretreatment for the determination of mercury in water and urine by flow-injection cold-vapour atomic absorption spectrometry. Anal. Chim. Acta 261 91-103. 

Fernandez, C., A.C.L. Conceicao, R. Rial-Otero, C. Vaz, and J.L. Capelo. 2006. Sequential flow injection analysis system on-line coupled to high intensity focused ultrasound Green methodology for trace analysis applications as demonstrated for the determination of inorganic and total mercury in waters and urine by cold vapor atomic absorption spectrometry. Anal. Chem. 78 2494-2499. 

Kagaya, S., Y. Kuroda, Y. Serikawa, and K. Hasegawa. 2004. Rapid determination of total mercury in treated waste water by cold vapor atomic absorption spectrometry in alkaline medium with sodium hypochlorite solution. Talanta 64 554-557. 

Ou, H., Y. Zhang, Q. Wu, J. Fang, and Y. Shu. 2004. Rapid determination of trace inorganic and total organic mercury in waste water by cold vapor atomic absorption spectrometry and pyrolysis atomic absorption spectrometry. Fenxi Ceshi Xuebao 23 68-70. 

European Standard. 2007. Water quality. Determination of mercury. Method using atomic absorption spectrometry. EN 1483. European Committee for Standardization, Brussels, Belgium. 

Gil, S., I. Lavilla, and C. Bendicho. 2006. Ultrasound-promoted cold vapor generation in the presence of formic acid for determination of mercury by atomic absorption spectrometry. Anal. Chem. 78 6260-6264. 

G. Tao, S. N. Willie, R. E. Sturgeon, Determination of total mercury in biological tissues by Bow injection cold vapour generation atomic absorption spectrometry following tetramethylammonium hydroxide digestion, Analyst, 123 (1998), 1215D1218. 

G. Schnitzer, A. Soubelet, C. Testu, C. Chafey, Comparison of open and closed focussed microwave digestions in view of total mercury determination by cold vapor atomic absorption spectrometry, Mikrochim. Acta, 119 (1995), 199-209. 

M. A. H. Hafez, I. M. M. Kenawy, M. A. Akl, R. R. Lashein, Preconcentration and separation of total mercury in environmental samples using chemically modified chlor-omethylated polystyrene-PAN (ion-exchanger) and its determination by cold vapor atomic absorption spectrometry, Talanta, 53 (2001), 749-760. 

F. Ubillus, A. Algeria, R. Barbera, R. Farre, M. J. Lagarda, Methylmercury and inorganic mercury determination in fish by cold vapour generation atomic absorption spectrometry, Food Chem., 71 (2000), 529-533. 

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