The present paper describes the ashing and atomization processes in silicon analysis by electrothermally atomised atomic absorption spectrometry(EAAAS) with an uncoat-ed graphite tube, a pyrolytically coated graphite ...The present paper describes the ashing and atomization processes in silicon analysis by electrothermally atomised atomic absorption spectrometry(EAAAS) with an uncoat-ed graphite tube, a pyrolytically coated graphite tube and a tungsten-coated graphitetube. The sensitivity and linear range of three graphite tubes were compared. By using optical temperature control accessory, the signals are enhanced by a factor of 2 and the germanium interferences in the determination of silicon are eliminated. The effects of time constant and carrier gas flow-rate on the determination of silicon were also tested. The sample can be directly analyzed in its aqueous solution without any pretreatment. The measurements of samples containing 0. 2 μg/mL and 0. 4 μg/mL silicon were run ten times and the variation coefficient is 4. 9% and 2.6%, respectively. The recovery tests for carboxyethyl germanium sesquioxide(Ge-132) synthesized and imported were performed, and the recoveries are 97. 0% and 110%, respectively. Keywords Carboxyethyl germanium sesquioxide, Electrothermally atomised atomic absorption spectrometry, Silicon展开更多
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
Non-thermal C/H/Ar plasmas are widely applied to carbonaceous material production and processing.In this work,plasma parameters and gaseous species of the atmospheric non-thermal C/H/Ar plasmas produced by an atmosphe...Non-thermal C/H/Ar plasmas are widely applied to carbonaceous material production and processing.In this work,plasma parameters and gaseous species of the atmospheric non-thermal C/H/Ar plasmas produced by an atmospheric-pressure DC arc discharge generator in CH_4/Ar were investigated.The voltage-current characteristics were measured for different CH_4/Ar ratios.Optical emission spectroscopy was employed to analyze the electron excitation temperature,gas temperature and electron density under various discharge conditions.The hydrocarbon molecules produced in the CH4/Ar plasmas were detected with photoionization mass spectrometry.The optical spectral results demonstrated that the electron excitation temperature was 0.4-1 eV,the gas temperature was 2800-4200 K and the electron density was in the range of（5-20）×10^15 cm^-3.The mass spectrum indicated that a variety of unsaturated hydrocarbons（C2H4,C3H6,C6H6,etc.） and several highly unsaturated hydrocarbons（C4H2,C5H6,etc.） were produced in the non-thermal arc plasmas.展开更多
In positive-ion fast atom bombardment (FAB) mass spectrometry, when mono- and di- saccharides are mixed with an appropriate amount of NH4Cl, a highly abundan peak [M+NH4]+appers in FAB mass spectra . From the adduct ...In positive-ion fast atom bombardment (FAB) mass spectrometry, when mono- and di- saccharides are mixed with an appropriate amount of NH4Cl, a highly abundan peak [M+NH4]+appers in FAB mass spectra . From the adduct ion [M+NH4]+, the molecular weights of mono- and di- saccharides can be determined definitively展开更多
文摘The present paper describes the ashing and atomization processes in silicon analysis by electrothermally atomised atomic absorption spectrometry(EAAAS) with an uncoat-ed graphite tube, a pyrolytically coated graphite tube and a tungsten-coated graphitetube. The sensitivity and linear range of three graphite tubes were compared. By using optical temperature control accessory, the signals are enhanced by a factor of 2 and the germanium interferences in the determination of silicon are eliminated. The effects of time constant and carrier gas flow-rate on the determination of silicon were also tested. The sample can be directly analyzed in its aqueous solution without any pretreatment. The measurements of samples containing 0. 2 μg/mL and 0. 4 μg/mL silicon were run ten times and the variation coefficient is 4. 9% and 2.6%, respectively. The recovery tests for carboxyethyl germanium sesquioxide(Ge-132) synthesized and imported were performed, and the recoveries are 97. 0% and 110%, respectively. Keywords Carboxyethyl germanium sesquioxide, Electrothermally atomised atomic absorption spectrometry, Silicon
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 National Natural Science Foundation of China(Nos.11035005,11475174,50876101)USTC-NSRL Association Funding(No.KY2090130001)
文摘Non-thermal C/H/Ar plasmas are widely applied to carbonaceous material production and processing.In this work,plasma parameters and gaseous species of the atmospheric non-thermal C/H/Ar plasmas produced by an atmospheric-pressure DC arc discharge generator in CH_4/Ar were investigated.The voltage-current characteristics were measured for different CH_4/Ar ratios.Optical emission spectroscopy was employed to analyze the electron excitation temperature,gas temperature and electron density under various discharge conditions.The hydrocarbon molecules produced in the CH4/Ar plasmas were detected with photoionization mass spectrometry.The optical spectral results demonstrated that the electron excitation temperature was 0.4-1 eV,the gas temperature was 2800-4200 K and the electron density was in the range of（5-20）×10^15 cm^-3.The mass spectrum indicated that a variety of unsaturated hydrocarbons（C2H4,C3H6,C6H6,etc.） and several highly unsaturated hydrocarbons（C4H2,C5H6,etc.） were produced in the non-thermal arc plasmas.
文摘In positive-ion fast atom bombardment (FAB) mass spectrometry, when mono- and di- saccharides are mixed with an appropriate amount of NH4Cl, a highly abundan peak [M+NH4]+appers in FAB mass spectra . From the adduct ion [M+NH4]+, the molecular weights of mono- and di- saccharides can be determined definitively
