Determination of mercury

X-Ray Methods. In x-ray fluorescence the sample containing mercury is exposed to a high iatensity x-ray beam which causes the mercury and other elements ia the sample to emit characteristic x-rays. The iatensity of the emitted beam is directly proportional to the elemental concentration ia the sample (22). Mercury content below 1 ppm can be detected by this method. X-ray diffraction analysis is ordinarily used for the quaUtative but not the quantitative determination of mercury. 

DETERMINATION OF MERCURY (Hg) IN NATURAL AND WASTE WATERS BY MEANS OF THE MILLENNIUM MERLIN ATOMIC FLUORESCENCE SPECTROFOTOMETER... 

Determination of mercury as mercury(II) thionalide Discussion. Thionalide C10H7 NH CO CH2 SH may be used for the quantitative precipitation of mercury(II) as Hg(C12H10ONS)2. Sulphate does not interfere. Attention is drawn to the following experimental points. 

A) Cold vapour technique. This procedure is strictly confined to the determination of mercury,45 which in the elemental state has an appreciable vapour pressure at room temperature so that gaseous atoms exist without the need for any special treatment. As a method for determining mercury compounds the procedure consists in the reduction of a mercury(II) compound with either... 

The use of the non-flame mercury cell (Section 21.6) is far more sensitive for the determination of mercury. 

Christopher SJ, Vander Pol SS, Pugh RS, Day RD, Becker PR. 2002. Determination of mercury in the eggs of Common Murres Uria Aalge) for the Seabird Tissue Archival and Monitoring Project. J Anal Atomic Spectrom 17 780-785. 

Biester H., Scholz C. Determination of mercury binding forms in contaminated soils Mercury pyrolysis versus sequential extractions. Environ Sci Technol 1997 31 233-239. 

Hedeishi and McLaughlin [457] have reported the application of the Zeeman effect for the determination of mercury. Atomic absorption and atomic fluorescence techniques using closed system reduction-aeration have been applied widely to determine mercury concentrations in natural samples [458-472]. 

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. 

Figure 5.12. Hg cold-trap preconcentration system for the determination of mercury by gas-phase absorption. Source [477]... 

Watling [491] has described an analytical technique for the accurate determination of mercury at picogram per litre levels in fresh and seawater. Mercury, released by tin (II) chloride reduction of water samples is amalgamated onto silver wool contained in quartz amalgamation tubes. The wool is then heated and the mercury thus released is flushed by argon into a plasma where it is excited. The emission signal thus produced results in a detection limit of 3 x 10 17 g and an analytical range 1 x 10 14 g-1 x 10"7 g. 

Wrembel [485] gives details of a procedure for the determination of mercury in seawater by low-pressure ring-discharge atomic emission spectrometry with electrolytic preconcentration on copper and platinum mesh electrodes. Between 40 5 (open sea) and 50 8 (shore area) xg/l mercury was found in Baltic sea waters. 

Wrembel and Pajak [486] evaporated mercury from natural water samples with argon and amalgamated the mercury with a gold foil. The mercury was excited in a ring-discharge plasma and determined by atomic emission spectroscopy. The method was applied to the determination of mercury in seawater in the range 0.01-1.0 xg/l. 

Foreback CC (1973) Some studies on the detection and determination of mercury, arsenic, and antimony in gas discharges. Thesis. University of South Florida... 

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. 

A number of workers have described methods for the determination of mercury in which the mercury is first reduced to the element or collected as the sulfide on a cadmium sulfide pad. It is then volatilized into a chamber for measurement. These techniques are extremely sensitive. Thillez108) recently described a procedure for urinary mercury in which the mercury is collected on platinum and then volatilized into an air stream. Rathje109) treated 2 ml of urine with 5 ml of nitric acid for 3 min, diluted to 50 ml, and added stannuous chloride to reduce the mercury to the element. A drop of Antifoam 60 was added and nitrogen was blown through the solution to carry the mercury vapor into a quartz end cell where it is measured. Six nanograms of mercury can be detected. Willis 93) employed more conventional methods to determine 0.04 ppm of mercury in urine by extracting it with APDC into methyl-n-amyl ketone. Berman n°) extracted mercury with APDC into MIBK to determine 0.01 ppm. 

Bishop, J.N., Taylor, L.A. and Neary, B.P. (1973) in The Determination of Mercury in Environment Samples, Ministry of the Environment, Ontario, Canada. 

Zheng AF, Chen JL, Wu GN et al (2009) Optimization of a sensitive method for the switch-on determination of mercury(II) in waters using rhodamine B capped gold nanoparticles as a fluorescence sensor. Microchim Acta 164 17-27... 

Determination of Mercury in Water by Cold Vapor AA Spectrometry... 

Since the introduction of the first fully automated laboratory-based mercury analysers in 1989, a number of other systems have been introduced. Around 20 different systems are available with varying levels of performance, and many claim to measure mercury at low levels. The analyst can therefore be forgiven if the determination of mercury is considered a trivial problem. Despite the various claims, the determination of low levels of mercury... 

SDS), and indeed SDS-catalysis of Hg " -catalyzed replacement of cyanides in [Fe(C1 6]" 1 1,10-phenanthroline has been proposed as an analytical method for the determination of mercury. ... 

The construction and behavior of a mixed binder carbon paste electrode containing dimethylglyoxime have been described [79]. Such an electrode was used for CSV determination of mercury(II) and other metal ions. They were accumulated at the electrode surface during preconcentration step and later reduced from their complexes in the cathodic step. 

The certification procedure for seven trace metals (Ba, Ca, Li, Mg, Mn, Na and Sr) in the certified reference material FEBS-1 (National Research Council Canada, Institute for National Measurement Standards, Ottawa, Canada) based on fish otolith matrix by isotope dilution - ICP-MS in comparison to ICP optical emission spectrometry and X-ray fluorescence analysis, is described by Sturgeon et al4X The isotope dilution technique is also employed for species analysis in biological systems,46 e.g., for the determination of mercury species in tuna material,54 or in aquatic systems using cold vapour ICP-MS.55... 

Concerning AFS, the atomiser can be a flame, plasma, electrothermal device or a special-purpose atomiser e.g. a heated quartz cell). Nowadays, commercially available equipment in AFS is simple and compact, specifically configured for particular applications e.g. determination of mercury, arsenic, selenium, tellurium, antimony and bismuth). Therefore, particular details about the components of the instrumentation used in AFS will not be given in this chapter. 

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. 

R. Puk and J. H. Weber, Determination of mercury (II), mono-methylmercury cation, dimethylmercury and diethylmercury by hydride generation, cryogenic trappling and atomic absorption spectrometric detection. Anal. Chim. Acta, 292(1-2), 1994, 175-183. 

G. A. Zachariadis and J. A. Stratis, Optimisation of cold vapour atomic absorption spectrometric determination of mercury with and without amalgamation by subsequent use of complete and fractional factorial designs with univariate and modified simplex methods, J. Anal. At. Speetrom., 6(3), 1991, 239-245. 

To recover gold from electronics, see J. W. Hill and T. A. Lear, Recovery of Gold from Electronic Scrap, J. Chem. Ed. 1988,65, 802. To remove Hg from gold, soak it in a 1 1 mixture of 0.01 M (NH4)2S208 and 0.01 M HNOj [T. Nomura and M. Fujisawa, Electrolytic Determination of Mercury(II) in Water with a Piezoelectric Quartz Crystal, Anal. Chim. Acta 1986, 182, 267]. 

D. L. Pfeil and A. Reed, Automating the Digestion and Determination of Mercury in a Variety of Environmental Sample Matrices, Am. Lab., March... 

S. E. Long and W. R. Kelly, Determination of Mercury in Coal by Isotope Dilution Cold-Vapor Generation Inductively Coupled Plasma Mass Spectrometry, Anal. Chem. 2002, 74, 1477. 

Determination of Mercury, Fluorine, Boron, and Selenium. The Determination of Mercury. A coal sample is decomposed by igniting a combustion bomb containing a dilute nitric acid solution under 24 atm of oxygen. After combustion, the bomb washings are diluted to a known volume, and mercury is determined by atomic absorption spectrophotometry using a flameless cold vapor technique. 

Procedures for the determination of 11 elements in coal—Sb, As, Br, Cd, Cs, Ga, Hg, Rb, Se, U, and Zn—by neutron activation analysis with radiochemical separation are summarized. Separation techniques include direct combustion, distillation, precipitation, ion exchange, and solvent extraction. The evaluation of the radiochemical neutron activation analysis for the determination of mercury in coal used by the Bureau of Mines in its mercury round-robin program is discussed. Neutron activation analysis has played an important role in recent programs to evaluate and test analysis methods and to develop standards for trace elements in coal carried out by the National Bureau of Standards and the Environmental Protection Agency. 

O Gorman et al. (19) used radiochemical NAA as a referee method in evaluating the determination of mercury by atomic absorption techniques. A commercial testing laboratory did the neutron activation analyses. 

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