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
An experimental setup was built up to carry out radio frequency (RF) inductively coupled plasma (ICP) and dielectric barrier discharge (DBD), and to depict the optical emission spectra (OES) of the discharges. OES fro...An experimental setup was built up to carry out radio frequency (RF) inductively coupled plasma (ICP) and dielectric barrier discharge (DBD), and to depict the optical emission spectra (OES) of the discharges. OES from argon ICP and DBD plasmas in visible and near ultraviolet region were measured. For argon ICP, the higher RF power input (higher than 500 W for our machine), the higher degree of argon plasma ionization. But that doesn't mean a higher mean electron energy. With the increase in the power input, the mean electron energy increases slightly, whereas the density of electron increases apparently On the contrary, argon DBD discharge behaves in the manner of a pulsed DC discharge on optical emission spectroscopy and V-I characteristics. DBD current is composed of a series of pulses equally spaced in temporal domain. The Kinetics of DBD emission strength is mainly governed by the frequency of the current pulse.展开更多
The ion line of 434.8 nm and atom line of 419.8 nm of Ar plasma produced by an inductively coupled plasma （ICP） were measured by optical emission spectroscopy and the influences from the working gas pressure, radio-...The ion line of 434.8 nm and atom line of 419.8 nm of Ar plasma produced by an inductively coupled plasma （ICP） were measured by optical emission spectroscopy and the influences from the working gas pressure, radio-frequency （RF） power and different positions in the discharge chamber on the line intensities were investigated in this study. It was found that the intensity of Ar atom line increased firstly and then saturated with the increase of the pressure. The line intensity of Ar^＋, on the other hand, reached a maximum value and then decreased along with the pressure. The intensity of the line in an RF discharge also demonstrated a jumping mode and a hysteresis phenomenon with the RF power. When the RF power increased to 400 W, the discharge jumped from the E-mode to the H-mode where the line intensity of Ar atom demonstrated a sudden increase, while the intensity of Ar^＋ ion only changed slightly. If the RF power decreased from a high value, e.g., 1000 W, the discharge would jump from the H-mode back to the E-mode at a power of 300 W. At this time the intensities of Ar and Ar^＋ lines would also decrease sharply. It was also noticed in this paper that the intensity of the ion line depended on the detective location in the chamber, namely at the bottom of the chamber the line was more intense than that in the middle of the chamber, but less intense than at the top, which is considered to be related to the capacitance coupling ability of the ICP plasma in different discharge areas.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This work is supported by the National Science Foundation of China No.19835030.
文摘An experimental setup was built up to carry out radio frequency (RF) inductively coupled plasma (ICP) and dielectric barrier discharge (DBD), and to depict the optical emission spectra (OES) of the discharges. OES from argon ICP and DBD plasmas in visible and near ultraviolet region were measured. For argon ICP, the higher RF power input (higher than 500 W for our machine), the higher degree of argon plasma ionization. But that doesn't mean a higher mean electron energy. With the increase in the power input, the mean electron energy increases slightly, whereas the density of electron increases apparently On the contrary, argon DBD discharge behaves in the manner of a pulsed DC discharge on optical emission spectroscopy and V-I characteristics. DBD current is composed of a series of pulses equally spaced in temporal domain. The Kinetics of DBD emission strength is mainly governed by the frequency of the current pulse.
基金supported by National Natural Science Foundation of China (Nos.50277003,10505005)
文摘The ion line of 434.8 nm and atom line of 419.8 nm of Ar plasma produced by an inductively coupled plasma （ICP） were measured by optical emission spectroscopy and the influences from the working gas pressure, radio-frequency （RF） power and different positions in the discharge chamber on the line intensities were investigated in this study. It was found that the intensity of Ar atom line increased firstly and then saturated with the increase of the pressure. The line intensity of Ar^＋, on the other hand, reached a maximum value and then decreased along with the pressure. The intensity of the line in an RF discharge also demonstrated a jumping mode and a hysteresis phenomenon with the RF power. When the RF power increased to 400 W, the discharge jumped from the E-mode to the H-mode where the line intensity of Ar atom demonstrated a sudden increase, while the intensity of Ar^＋ ion only changed slightly. If the RF power decreased from a high value, e.g., 1000 W, the discharge would jump from the H-mode back to the E-mode at a power of 300 W. At this time the intensities of Ar and Ar^＋ lines would also decrease sharply. It was also noticed in this paper that the intensity of the ion line depended on the detective location in the chamber, namely at the bottom of the chamber the line was more intense than that in the middle of the chamber, but less intense than at the top, which is considered to be related to the capacitance coupling ability of the ICP plasma in different discharge areas.
