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Sun H.-L.,Henan Province Rock & Mineral Testing Center | Sun H.-L.,Ministry of Land and Resources Key Laboratory of Precious Metals Analysis Technology | Wang L.,Henan Province Rock & Mineral Testing Center | Wang L.,Ministry of Land and Resources Key Laboratory of Precious Metals Analysis Technology | And 6 more authors.
Yejin Fenxi/Metallurgical Analysis | Year: 2015

The sample was decomposed by KClO3 in HCl-H2O2 wet system. It not only overcame the influence of NO3 - to platinum and palladium, but also greatly enhanced the decomposition capacity. After decomposition in HCl-H2O2-KClO3 high-efficiency wet system, the sample solution was separated and enriched by activated carbon-717 anion exchange resin mixed adsorbent in 10% (V/V) HCl medium. The influence of interference elements could be effectively eliminated. The Pt 265.945{127} nm, Pd 340.458{99} nm and Au 242.795{139} nm were used as analytical lines. The determination method of platinum, palladium and gold in geological samples by inductively coupled plasma atomic emission spectrometry (ICP-AES) was established. The detection limit of platinum, palladium and gold was 0.015, 0.012 and 0.005 1 μg/g, respectively. The low limit of determination was 0.050, 0.040 and 0.017 μg/g, respectively. The platinum, palladium and gold in standard geological samples were determined according to the experimental method, and the relative standard deviations (RSD, n=10) were less than 6.7%. The found results were consistent with the certified values. © 2015, Central Iron and Steel Research Institute. All right reserved.


Wu B.-C.,Ministry of Land and Resources Key Laboratory of Precious Metals Analysis Technology | Wu B.-C.,Henan Province Rock and Mineral Testing Center | Yu Y.-H.,Ministry of Land and Resources Key Laboratory of Precious Metals Analysis Technology | Yu Y.-H.,Henan Province Rock and Mineral Testing Center | And 8 more authors.
Yejin Fenxi/Metallurgical Analysis | Year: 2016

The tungsten ore and molybdenum ore are refractory and usually dissolved by alkali fusion method. However, a lot of sodium ions in the flux would be introduced into sample solution and lead to high salinity with the pretreatment by alkali fusion. The high salinity could cause matrix interference and cone-hole blocking, which is disadvantageous to determination of trace rare earth elements by inductively coupled plasma mass spectrometry (ICP-MS). In order to solve this problem, the sample was fused with NaOH and Na2O2 at high temperature followed by leaching and filtration with hot water. Then the rare earth elements were enriched into rare earth hydroxide precipitates, realizing the separation from much sodium and other metallic ions such as potassium, tungsten and molybdenum. The precipitate was dissolved with tartaric acid-HCl system. After dilution, the content of rare earth elements in tungsten ore and molybdenum ore was determined by ICP-MS. The results showed that 0.500 0 g of sample could be fully decomposed with 3.0 g of NaOH and 1.5 g of Na2O2 in muffle furnace at 700℃ for 20 min. The mass spectrometry interference could be eliminated by selecting proper isotopes and mathematic correction methods. The analytical signal drift and matrix effect could be effectively monitored and corrected with 10 μg/L 103Rh as internal standard. Under the optimal conditions, the correlation coefficients of calibration curves of all elements were all higher than 0.999 5. The detection limit of method was 0.004-0.08 μg/g. The experimental method was applied to the determination of rare earth elements in component analysis certified reference materials of molybdenum ore and tungsten ore. The absolute values of logarithm error (ΔlgC) between the results and the certified values were all less than 0.1 (the requirements according to industrial standard of DZ/T 0130-2006 for geology and mineral resources). The relative standard deviations (RSD, n=6) were all less than 5%. © 2016, CISRI Boyuan Publishing Co., Ltd. All right reserved.


Liu J.,Henan Province Rock and Mineral Testing Center | Liu J.,Ministry of Land and Resources Key Laboratory of Precious Metals Analysis Technology | Yan H.-L.,Henan Province Rock and Mineral Testing Center | Yan H.-L.,Ministry of Land and Resources Key Laboratory of Precious Metals Analysis Technology | And 8 more authors.
Yejin Fenxi/Metallurgical Analysis | Year: 2016

After the sample was dissolved in high pressure sealed system, a direct determination method of Au, Ag, Pt and Pd in geological samples was established by inductively coupled plasma mass spectrometry (ICP-MS). The experimental results showed that, 10.00 g of geological samples could be fully dissolved by adding 30 mL of HCl, 5.0 mL of H2O2 and 2.0 g of KClO3 in 200 mL high pressure sealed tank, which was put in constant temperature digital drying oven at 160℃ for 6 h. The sample digestion solution was separated and enriched with novel composite adsorbent composed of activated carbon, modified activated carbon and 717 anion exchange resin. Then the mass spectrometry interference was eliminated by selecting proper isotopes or mathematic correction. Consequently, the determination of Au, Ag, Pt and Pd in geological samples was realized by ICP-MS. The correlation coefficients of calibration curves of Au, Ag, Pt and Pd were not less than 0.999 5. The detection limit of Au, Ag, Pt and Pd was 0.097, 0.14, 0.17 and 0. 082 ng/g, respectively. The proposed method was applied to the determination of Au, Ag, Pt and Pd in geochemical primary reference materials of platinum family element, and the results were consistent with the certified values. The relative standard deviation (RSD, n=12) was not more than 14. 2%. The experimental method was applied to the determination of Au, Ag, Pt and Pd in geochemical primary reference materials and actual samples, and the recoveries were between 92% and 110%. © 2016, CISRI Boyuan Publishing Co., Ltd. All right reserved.

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