Centrifugation metal analysis

The reaction mixture can either be crystallised, centrifuged, and dried, or spray-dried and cyclone-separated to produce a fine crystalline powder having a particle size of 50 p.m. Metal analysis of the AP produced by this method is reported to be less than 0.02 p.g/g. 

Filtration of the catalytic mixture using pore membrane filters or filter aids allows the distinction between soluble and insoluble catalysts. Further catalytic activity analysis from the solution and insoluble residue can give information about the state of the real catalyst. In turn, centrifugation can be appropriated to separate metal NPs from the catalytic solutions, due to their high molecular weight and density, and thus to be separated from molecular species. 

Shipboard analysis for the sampling of trace metals in seawater has been discussed by Schuessler and Kremling [2] and Dunn et al. [3]. Teasdale et al. have reviewed methods for collection of sediment pore-waters using in situ dialysis samples [4]. Bufflap and Allen [5] compared centrifugation, squeezing, vacuum filtration, and dialysis methods for sediment pore-water sampling. 

Many metals in seawater can be preconcentrated for analysis by coprecipitation with Ga(OH)3. A 200-p.L HC1 solution containing 50p,g of Ga3+ is added to 10.00 mL of the seawater. When the pH is brought to 9.1 with NaOH, a jellylike precipitate forms. After centrifugation to pack the precipitate, the water is removed and the gel is washed with water. Then the gel is dissolved in 50 p,L of 1 M HN03 and aspirated into an inductively coupled plasma for atomic emission analysis. The preconcentration factor is 10 mL/50 p,L = 200. The figure shows elemental concentrations in seawater as a function of depth near hydrothermal vents. 

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. 

Concentrations were determined by atomic absorption (AA) with a Perkin-Elmer Model 2380. For amounts of sorbed metals, the solid was treated with 0.01 M HN03 for 30 min followed by centrifugation and AA analysis of the aqueous layer. 

Table 5.19 Results of analysis of wear oil obtained from a local automobile factory using a slurry method and yttrium as internal standard. The results before and after centrifugations are indicative of suspended and dissolved metal content...

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