Decomposition of Some Skarn-Rock Samples in Neutral and Basic Molten Potassium Nitrate for the Extraction and Determination of Iron

1996 ◽  
Vol 49 (2) ◽  
pp. 261 ◽  
Author(s):  
JK Mujumba ◽  
BD James ◽  
SA Tariq

Five skarn -rock samples were heated with KNO3 and with a solution of 5% KOH in KNO3 for 2 h at 450°C. The decomposed samples were cooled, dissolved in water and filtered. Iron was extracted from each residue as well as from the original samples by hot conc. HCl , and determined by atomic absorption spectroscopy. These results were compared with the known (X-ray fluorescence) total iron content of the original samples. The amount of iron extracted with HCl from the skarn samples was 3-11% lower, while that extracted after heating with KNO3 alone was 2-4% lower, than the amount present according to the X-ray fluorescence results. However, the amount of iron extracted from the samples treated with a solution of KOH in KNO3 was comparable to that determined by X-ray fluorescence.

1998 ◽  
Vol 81 (1) ◽  
pp. 89-92 ◽  
Author(s):  
Nancy M Hepp

Abstract An X-ray fluorescence (XRF) method was developed for determining manganese in FD&C Blue No. 1 from simply prepared pressed pellets. Results were compared with those of atomic absorption spectroscopy (AAS) of acid-digested or ashed samples. Levels of manganese determined by XRF and AAS were equivalent. The limit of detection (3σ) for the XRF method was 3µg manganese/g dye. The 95% confidence interval at the specification level was 100 ± 10 μg manganese/g dye


2008 ◽  
Vol 23 (6) ◽  
pp. 1764-1775 ◽  
Author(s):  
Fernando Vereda ◽  
Juan de Vicente ◽  
Roque Hidalgo-Álvarez

We report the fabrication of micron-sized rodlike particles of nonstoichiometric Co and Ni ferrites by aging coprecipitated Fe(OH)2 and M(OH)2—where M is either Ni or Co—at 90 °C in the presence of an external magnetic field (B ≈ 405 mT). Potassium nitrate was used as a mild oxidant. Resultant particles were analyzed by means of electron microscopy, x-ray powder diffraction (XRD), magnetometry, energy dispersive x-ray (EDX) spectrometry, and atomic absorption spectroscopy. Rodlike particles of both types of ferrite exhibited a relatively uniform thickness, an average aspect ratio close to 10, and have a spinel crystalline structure. EDX spectrometry and atomic absorption spectroscopy confirmed the incorporation of Ni2+ and Co2+ in the respective ferrite particles. The incorporation of Co2+ led to non-negligible remanence and coercivity. The incorporation of Ni2+ led to a lower saturation magnetization, whereas the remanence and coercivity of the Ni ferrite were very low, still typical of a soft ferrimagnetic material. The mechanism of formation of the rodlike particles was investigated by the time-dependent observation of growing Ni ferrite rods.


1974 ◽  
Vol 57 (6) ◽  
pp. 1260-1264
Author(s):  
Samuel Ng ◽  
Maurice Munroe ◽  
William McSharry

Abstract An atomic absorption spectrophotometry method for the determination of selenium in animal feed premixes is described. The method involves digesting the samples by heating with perchloric acid and hydrogen peroxide. No pre-concentration or separation is required other than filtering the insoluble material remaining after digestion. Concentrations from 0.0057 to 0.42% selenium were measured. The relative standard deviation over this range averaged 4.6%. A matrix effect, which could be overcome by either preparing the standards with a matrix or using the standard addition technique, was noted at ≤0.02% selenium. The results obtained by each method and by x-ray fluorescence are shown and compared with the claimed selenium content. When the matrix effect is overcome, results by atomic absorption spectroscopy and x-ray fluorescence agree within 15% or better at all levels.


1996 ◽  
Vol 79 (5) ◽  
pp. 1189-1190 ◽  
Author(s):  
Nancy M Hepp

Abstract An X-ray fluorescence spectrometry (XRF) method was developed and validated for determination of chromium in FD&C Blue No. 1. Results of this analysis were compared with those obtained with an atomic absorption spectroscopy (AAS) method currently used by the U.S. Food and Drug Administration. Levels of Cr, as determined by the XRF and AAS methods, were comparable. The limit of quantitation for the XRF method is 4 μg Cr/g. The predicted 95% confidence interval at the specification level is 50 ± 5 μg/g.


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