An improved analytical method to determine the content of 52 major, minor and trace elements in marine geological samples, using a HF-HCl-HNO_3 acid system with a high-pressure closed digestion method(HPCD), is stud...An improved analytical method to determine the content of 52 major, minor and trace elements in marine geological samples, using a HF-HCl-HNO_3 acid system with a high-pressure closed digestion method(HPCD), is studied by an inductively coupled plasma optical emission spectrometry(ICP-OES) and an inductively coupled plasma mass spectrometry(ICP-MS). The operating parameters of the instruments are optimized, and the optimal analytical parameters are determined. The influences of optical spectrum and mass spectrum interferences, digestion methods and acid systems on the analytical results are investigated. The optimal spectral lines and isotopes are chosen, and internal standard element of rhodium is selected to compensate for matrix effects and analytical signals drifting. Compared with the methods of an electric heating plate digestion and a microwave digestion, a high-pressure closed digestion method is optimized with less acid, complete digestion,less damage for digestion process. The marine geological samples are dissolved completely by a HF-HCl-HNO_3 system, the relative error(RE) for the analytical results are all less than 6.0%. The method detection limits are 2–40μg/g by the ICP-OES, and 6–80 ng/g by ICP-MS. The methods are used to determine the marine sediment reference materials(GBW07309, GBW07311, GBW07313), rock reference materials(GBW07103, GBW07104,GBW07105), and cobalt-rich crust reference materials(GBW07337, GBW07338, GBW07339), the obtained analytical results are in agreement with the certified values, and both of the relative standard deviation(RSD) and the relative error(RE) are less than 6.0%. The analytical method meets the requirements for determining 52 elements contents of bulk marine geological samples.展开更多
The safety of rail is very important for the development of high speed railway, and it is necessary to investigate the features of inner cracks in rail. In order to obtain the features of Acoustic Emission (AE) sour...The safety of rail is very important for the development of high speed railway, and it is necessary to investigate the features of inner cracks in rail. In order to obtain the features of Acoustic Emission (AE) sources of inner cracks in rail, AE sources with different types, depths and propagation distances are examined for crack in rail. The finite element method is utilized to model the rail with cracks and the results of experiment demonstrate the effectiveness of this model. Wavelet transform and Rayleigh-Lamb equations are utilized to extract the features of crack AE sources. The results illustrate that the intensity ratio among AE modes can identify the AE source types and the AE sources with different frequencies in rail. There are uniform AE mode features existing in the AE signals from AE sources in rail web, however AE signals from AE sources in rail head and rail base have the complex and unstable AE modes. Different AE source types have the different propagation features in rail. It is helpful to understand the rail cracks and detect the rail cracks based on the AE technique.展开更多
基金The China Ocean Mineral Resources Research and Development Association Research Program of the State Oceanic Administration of China under contract No.DY125-13-R-07the National Natural Science Foundation of China under contract Nos 41322036 and 41230960+1 种基金the Shandong Provincial Natural Science Foundation of China under contract No.ZR2014DP009the Special Basic Research Funds for Central Public Research Institutes for The First Institute of Oceanography,State Oceanic Administration of China under contract Nos GY0213G06 and GY02-2012G35
文摘An improved analytical method to determine the content of 52 major, minor and trace elements in marine geological samples, using a HF-HCl-HNO_3 acid system with a high-pressure closed digestion method(HPCD), is studied by an inductively coupled plasma optical emission spectrometry(ICP-OES) and an inductively coupled plasma mass spectrometry(ICP-MS). The operating parameters of the instruments are optimized, and the optimal analytical parameters are determined. The influences of optical spectrum and mass spectrum interferences, digestion methods and acid systems on the analytical results are investigated. The optimal spectral lines and isotopes are chosen, and internal standard element of rhodium is selected to compensate for matrix effects and analytical signals drifting. Compared with the methods of an electric heating plate digestion and a microwave digestion, a high-pressure closed digestion method is optimized with less acid, complete digestion,less damage for digestion process. The marine geological samples are dissolved completely by a HF-HCl-HNO_3 system, the relative error(RE) for the analytical results are all less than 6.0%. The method detection limits are 2–40μg/g by the ICP-OES, and 6–80 ng/g by ICP-MS. The methods are used to determine the marine sediment reference materials(GBW07309, GBW07311, GBW07313), rock reference materials(GBW07103, GBW07104,GBW07105), and cobalt-rich crust reference materials(GBW07337, GBW07338, GBW07339), the obtained analytical results are in agreement with the certified values, and both of the relative standard deviation(RSD) and the relative error(RE) are less than 6.0%. The analytical method meets the requirements for determining 52 elements contents of bulk marine geological samples.
基金supported by the China Scholarship Council,the National Natural Science Foundation of China(61171197,61201307,61371045)the Innovation Funds of Harbin Institute of Technology(Grant IDGA18102011)the Promotive Research Fund for Excellent Young and Middle-Aged Scientisits of Shandong Province(BS2010DX001)
文摘The safety of rail is very important for the development of high speed railway, and it is necessary to investigate the features of inner cracks in rail. In order to obtain the features of Acoustic Emission (AE) sources of inner cracks in rail, AE sources with different types, depths and propagation distances are examined for crack in rail. The finite element method is utilized to model the rail with cracks and the results of experiment demonstrate the effectiveness of this model. Wavelet transform and Rayleigh-Lamb equations are utilized to extract the features of crack AE sources. The results illustrate that the intensity ratio among AE modes can identify the AE source types and the AE sources with different frequencies in rail. There are uniform AE mode features existing in the AE signals from AE sources in rail web, however AE signals from AE sources in rail head and rail base have the complex and unstable AE modes. Different AE source types have the different propagation features in rail. It is helpful to understand the rail cracks and detect the rail cracks based on the AE technique.