Manganese analytical determination

The application of the Chelex 100 resin separation and preconcentration, with the direct use of the resin itself as the final sample for analysis, is an extremely useful technique. The elements demonstrated to be analytically determinable from high salinity waters are cobalt, chromium, copper, iron, manganese, molybdenum, nickel, scandium, thorium, uranium, vanadium, and zinc. The determination of chromium and vanadium by this technique offers significant advantages over methods requiring aqueous final forms, in view of their poor elution reproducibility. The removal of sodium, chloride, and bromide allows the determination of elements with short and intermediate half-lives without radiochemistry, and greatly reduces the radiation dose received by personnel. This procedure was successfully applied in a study of... 

Table 2. 16 Analytical determinations of manganese (percentage mass) in steel carried out in four different laboratories based on three analytical principles.

Identification of sources of analytical bias in method development and method validation is another very important application of reference materials in geochemical laboratories. USGS applied simplex optimization in establishing the best measurement conditions when the ICP-AES method was introduced as a substitute for AAS in the rapid rock procedure for major oxide determinations (Leary et al. 1982). The optimized measurement parameters were then validated by analyzing a number of USGS rock reference samples for which reference values had been established first by classical analyses. Similar optimization of an ICP-AES procedure for a number of trace elements was validated by the analysis of U S G S manganese nodule P-i (Montaser et al. 1984). 

Caroli S, Forte G, Iamiceu AL, Galoppi B 1999) Determination of essential and potentially toxic trace elements in honey by inductively coupled plasma-based techniques. Talanta 50 327-336. Chiswell B, Johnson D (1994) Manganese. In Seiler HG, Sigel A, Sigel H, eds. Handbook on metals in clinical and analytical chemistry. Dekker, New York. 

Graphite-furnace atomic absorption spectrometry, although element-selective and highly sensitive, is currently unable to directly determine manganese at the lower end of their reported concentration ranges in open ocean waters. Techniques that have been successfully employed in recent environmental investigations have thus used a preliminary step to concentrate the analyte and separate it from the salt matrix prior to determination by atomic absorption spectrometry. 

Statham [448] has optimised a procedure based on chelation with ammonium dithiocarbamate and diethylammonium diethyldithiocarbamate for the preconcentration and separation of dissolved manganese from seawater prior to determination by graphite furnace atomic absorption spectrometry. Freon TF was chosen as solvent because it appears to be much less toxic than other commonly used chlorinated solvents, it is virtually odourless, has a very low solubility in seawater, gives a rapid and complete phase separation, and is readily purified. The concentrations of analyte in the back-extracts are determined by graphite furnace atomic absorption spectrometry. This procedure concentrates the trace metals in the seawater by a factor of 67.3. 

The luminol reaction has also been used for the CL determination of organic substances such as penicillins [32] and tartrate ion [30] in pharmaceutical preparations by their inhibitory effect on the luminol-iodine and luminol-periodate-manganese(II)-TEA system, respectively. As can be seen from Table 1, the results were quite satisfactory. In the indirect determination of penicillins by their inhibitory effect on the luminol-iodine system, the stopped-flow technique improves the accuracy and precision of the analytical information obtained, and also the sample throughput [32], Thus, in only 2-3 s one can obtain the whole CL signal-versus-time profile and calculate the three measured parameters formation and... 

With XPS it is possible to obtain good analytical information on the amount of metal adsorbed and, in favourable cases, to identify the chemical form of that metal. Oxidation states are readily determined and it can be shown, for example, that adsorption of Co(II) on manganese oxides results in oxidation to Co(III) (38,39), whereas adsorption of Co(II) on zirconia and alumina leads to the formation of cobalt(II) hydroxide (40). With Y-type zeolites hexaaquacobalt(II) is adsorbed as Co(II), and cobalt(III) hexaammlne is adsorbed as Co(III). The XPS spectrum of Co(II) adsorbed on chlorite was consistent with the presence of the hexaaquacobalt(II) ion for pH 3-7 and indicated that no cobalt(II) hydroxide was present (41). With kaollnlte and llllte, Co is adsorbed as Co(II) over the pH range 3-10 (39,42), it being bound as the aqua ion below pH 6 and as the hydroxide above pH 8. Measurements involving Pb have... 

The optical emission spectrum of technetium is uniquely characteristic of the element " with a few strong lines relatively widely spaced as in the spectra of manganese, molybdenum and rhenium. Twenty-five lines are observed in the arc and spark spectra between 2200 and 9000 A. Many of these lines are free from ruthenium or rhenium interferences and are therefore useful analytically. Using the resonance lines of Tc-I at 4297.06, 4262.26, 4238.19, and 4031.63 A as little as 0.1 ng of technetium can be reliably determined. 

Oxime 2 has been extensively used only as an analytical reagent (determination of manganese by photometry), jet-fuel additive and more recently in polymer synthesis d . 

Copper, Chromium, Manganese, and Nickel. The analytical method for determining copper, chromium, manganese, and nickel involves digesting the coal with nitric and perchloric acids, fusing the residue with lithium metaborate, and determining the combined digestion and leach solutions by atomic absorption spectrophotometry. Since there is no standard material to analyze for the construction of calibration curves, the standard additions method is used for the assay. While this method increases the time required for analysis, it helps to eliminate the effect of the matrix. 

Conditioning of the manganese oxide suspension with each cation was conducted in a thermostatted cell (25° 0.05°C.) described previously (13). Analyses of residual lithium, potassium, sodium, calcium, and barium were obtained by standard flame photometry techniques on a Beckman DU-2 spectrophotometer with flame attachment. Analyses of copper, nickel, and cobalt were conducted on a Sargent Model XR recording polarograph. Samples for analysis were removed upon equilibration of the system, the solid centrifuged off and analytical concentrations determined from calibration curves. In contrast to Morgan and Stumm (10) who report fairly rapid equilibration, final attainment of equilibrium at constant pH, for example, upon addition of metal ions was often very slow, in some cases of the order of several hours. 

Analytical Chemical Data for Natural Waters. While elemental compositions of various natural waters usually can be determined with good reliability, analytical methods to distinguish between free and complex-bound species, oxidized and reduced forms, simple and polynuclear metal ion forms, and even between dissolved and colloidal or suspended phases are often lacking. Data on the nature and amounts of the individual substances which make up the total concentrations of organic material found in different natural waters are not yet extensive. These analytical deficiencies relate almost solely to the highly reactive, non-conservative elements—e.g., iron, manganese, phosphorus, carbon, nitrogen, aluminum, and other metal ions. 

Dong et al. [ 13] evaluated sampling and analytical errors for the determination of manganese in soils, and no doubt the conclusions reached in this work could be applied to other elements. 

Chow, T. J., and C. R. McKinney Mass spectrometric determination of lead in manganese nodules. Analytic. Chem. 30, 1499 (1958). 

Brown AJ, Lenehan CE, Francis PS, Dunstan DE, Barnett NW. Soluble manganese(IV) as a chemiluminescence reagent for the determination of opiate alkaloids, indoles and analytes of forensic interest. Talanta 2007 71 1951-7. 

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