Henan Province Rock and Mineral Testing Center

Zhengzhou, China

Henan Province Rock and Mineral Testing Center

Zhengzhou, China

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Cao L.-F.,Henan Province Rock and Mineral Testing Center | Cao L.-F.,Key Laboratory of Precious Metals Analysis and Exploration Technology | Lian W.-L.,Henan Province Rock and Mineral Testing Center | Lian W.-L.,Key Laboratory of Precious Metals Analysis and Exploration Technology | And 2 more authors.
Yejin Fenxi/Metallurgical Analysis | Year: 2014

The sample was decomposed with hydrofluoric acid, hydrochloric acid, nitric acid and perchloric acid. Then, the content of CaO, MgO, Al2O3, Fe2O3, TiO2, K2O and Na2O in potash feldspar was simultaneously determined by inductively coupled plasma atomic emission spectrometry (ICP-AES). The analysis lines for testing elements and the method for background correction were selected. The effect of nebulization gas flow (1.0, 0.6, 0.5 and 0.4 L/min) on the spectral intensity, determination precision and calibration curve linearity of potassium, sodium, calcium, magnesium, aluminum, iron and titanium was investigated. The results showed that the determination precision of elements was best when the nebulization gas flow was 0.4 L/min and 0.5 L/min. The linear correlation coefficients of calibration curves were all higher than 0.999. However, the spectral intensities of elements were highest when the nebulization gas flow was 0.5 L/min. Therefore, the nebulization gas flow was selected as 0.5 L/min. The proposed method was applied to the determination of six components (CaO, MgO, Al2O3, Fe2O3, TiO2, K2O and Na2O) in certified reference materials of potash feldspar (GBW03116). The relative error (RE) between found results and certified values was between -3.64% and 4.26%. The relative standard deviation (RSD, n=11) was 0.76%-4.2%. ©, 2014, 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.


Chen J.,Henan Province Rock and Mineral Testing Center | Chen J.,Key Laboratory of Ministry and Resources Analysis and Exploration of Precious Metals
Yejin Fenxi/Metallurgical Analysis | Year: 2015

The sample was prepared with powder pressed pellet method. The relationship between fluorescence intensity and content of niobium and tantalum in geological samples during the determination by X-ray fluorescence spectrometry (XRF) was discussed. The determination conditions of low content niobium and tantalum were optimized. The detection limit of niobium and tantalum was 1.0 μg/g and 3.1 μg/g, respectively. The precision test was conducted by standard sample of stream sediment (GBW07311). The relative standard deviations (RSD, n=10) of determination results of niobium and tantalum were less than 2.0%. The proposed method was applied to the analysis of geological samples, and the found results were consistent with those obtained by inductively coupled plasma mass spectrometry (ICP-MS). When the content of niobium in geological sample was high, the spectral intensity of niobium decreased at peak value with concavity, which was due to the overflow of counting rate caused by the excessive content of niobium. As a result, the element showed self-absorption phenomenon. This problem was solved in experiments by selecting low tube voltage and tube current (40 kV-40 mA). This condition was applicable for the test of large amount samples. If the conventional tube voltage and tube current (50 kV-60 mA) were used, the method was applicable for the simultaneous determination of multiple elements in few amount of samples using Nb-Kβ(I) as analytical line. For the analysis of high content niobium and tantalum, the found results were consistent with those obtained by gravimetric method. The proposed method could meet the analysis requirements of niobium and tantalum in geological samples with different contents. ©, 2015, Central Iron and Steel Research Institute. All right reserved.


Gao Z.-J.,Henan Province Rock and Mineral Testing Center | Gao Z.-J.,Key Laboratory of Ministry and Resources Analysis and Exploration of Precious Metals | Chen J.,Henan Province Rock and Mineral Testing Center | Chen J.,Key Laboratory of Ministry and Resources Analysis and Exploration of Precious Metals | And 4 more authors.
Yejin Fenxi/Metallurgical Analysis | Year: 2015

The certified reference materials of soil, stream sediment, rock, iron ore and bauxite were prepared by fusion method for the fitting of calibration curve. The rapid analysis method for the simultaneous determination of major and minor components (SiO2, Al2O3, Fe2O3, TiO2, K2O, Na2O, CaO, MgO, P2O5 and MnO) in silicate and bauxite by X-ray fluorescence spectrometry(XRF) was established. The fusion conditions of samples were obtained as follows: the sample was uniformly mixed with lithium tetraborate-lithium metaborate (mass ratio of 67:33) with the dilution ratio of 1:10; then, 2 mL of 500 g/L NH4NO3 solution and 0.5 mL of 300 g/L NH4Br solution were added; the sample was pre-oxidized at 700℃ followed by fusion at 1100℃. The proposed method solved the following problems: each ore sample required one set of analysis method; the geological samples with various types could not be determined simultaneously. The components in certified reference material of bauxite (GBW07178 and GBW07179) were determined by proposed method. The relative standard deviation (RSD, n=12) was less than 5%. The relative error (RE) was less than 10%. The proposed method was also applied to the determination of silicate and bauxite samples, and the found results were consistent with those obtained by wet method. ©, 2015, Central Iron and Steel Research Institute. All right reserved.

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