The rapid quantitative analysis of nitrogen in steel with optical emission spectrometry is described.The problems about the selection of spectral line for the determination of nitrogen,the analytical conditions of nit...The rapid quantitative analysis of nitrogen in steel with optical emission spectrometry is described.The problems about the selection of spectral line for the determination of nitrogen,the analytical conditions of nitrogen,the preparation of analytical sample,the effect of co-existing element and the calibration curve of nitrogen are discussed.The analytical range of nitrogen is 0.000 5%to 0.30%,the limit of detection is 0.000 374%,the analytical time is less than 2 min(including the preparation of sample and the exciting sample for two times).Nitrogen in steel is simultaneously determined with alloy elements and acid soluble/insoluble compounds of aluminium.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
Electron density （Ne） in a glow discharge plasma for the surface alloying technique is diagnosed by optical emission spectrometry （OES）. With CH4 as the feeding gas, Ne is obtained by comparing the Hβ spectrum ac...Electron density （Ne） in a glow discharge plasma for the surface alloying technique is diagnosed by optical emission spectrometry （OES）. With CH4 as the feeding gas, Ne is obtained by comparing the Hβ spectrum according to the Stark broadening effect. It is noticed that Ne varies with the working pressures （30 Pa to 70 Pa） and cathode voltages （500 V to 1000 V）, respectively. Due to an abnormal glow discharge, Ne is between 1. 71 × 10^15 /cm^3 to 6.64 × 10^15 /cm^3 and increases rapidly with working gas pressures and cathode voltages. The results show that OES is a useful method to measure the plasma parameters in a surface alloying glow discharge plasma.展开更多
An environmentally friendly,low power consuming,sensitive and compact mercury analyzer was developed for the determination of mercury in water samples by integrating a thin film dielectric barrier discharge induced co...An environmentally friendly,low power consuming,sensitive and compact mercury analyzer was developed for the determination of mercury in water samples by integrating a thin film dielectric barrier discharge induced cold vapor reactor and a dielectric barrier discharge optical emission spectrometer into a small polymethyl methacrylate plate（10.5 cm length×8.0 cm width×1.2 cm height）.Mercury cold vapor was generated when standard or sample solutions with or without formic acid were introduced to the reactor to form thin film liquid and exposed to microplasma irradiation and subsequently separated from the liquid phase for transport to the microplasma and detection of its atomic emission.Limits of detection of 0.20 μg L^-1 and 2.6 μg L^-1 were obtained for the proposed system using or not using formic acid,respectively.Compared to the conventional microplasma optical emission spectrometry used for mercury analysis,this system not only retains the good limit of detection amenable to the determination of mercury in real samples,but also reduces power consumption,eliminates the generation of hydrogen and avoids the use of toxic or unstable reductant.Method validation was demonstrated by analysis of a certified reference material of water sample and three real water samples with good spike recoveries（88-102%）.展开更多
The capacitively coupled radio frequency（CCRF）plasma has been widely used in various fields.In some cases,it requires us to estimate the range of key plasma parameters simpler and quicker in order to understand the ...The capacitively coupled radio frequency（CCRF）plasma has been widely used in various fields.In some cases,it requires us to estimate the range of key plasma parameters simpler and quicker in order to understand the behavior in plasma.In this paper,a glass vacuum chamber and a pair of plate electrodes were designed and fabricated,using 13.56 MHz radio frequency（RF）discharge technology to ionize the working gas of Ar.This discharge was mathematically described with equivalent circuit model.The discharge voltage and current of the plasma were measured atdifferent pressures and different powers.Based on the capacitively coupled homogeneous discharge model,the equivalent circuit and the analytical formula were established.The plasma density and temperature were calculated by using the equivalent impedance principle and energy balance equation.The experimental results show that when RF discharge power is 50–300 W and pressure is 25–250 Pa,the average electron temperature is about 1.7–2.1 e V and the average electron density is about 0.5？×10^17–3.6？×10^17m^-3.Agreement was found when the results were compared to those given by optical emission spectroscopy and COMSOL simulation.展开更多
A diode-pumped solid-state laser （DPSSL） with a high energetic stability and long service life is applied to ablate the steel samples instead of traditional Nd：YAG laser pumped by a xenon lamp, and several factors,...A diode-pumped solid-state laser （DPSSL） with a high energetic stability and long service life is applied to ablate the steel samples instead of traditional Nd：YAG laser pumped by a xenon lamp, and several factors, such as laser pulse energy, repetition rate and argon flow rate, that influence laser-induced breakdown spectroscopy （LIBS） analytical performance are investigated in detail. Under the optimal experiment conditions, the relative standard deviations for C, Si, Mn, Ni, Cr and Cu are 3.3%-8.9%, 0.9%-2.8%, 1.2%-4.1%, 1.7%-3.0%, 1.1%-3.4% and 2.5%-8.5%, respectively, with the corresponding relative errors of 1.1%-7.9%, 1.0%-6.3%, 0.4%-3.9%, 1.5%-6.3%, 1.2%-4.0% and 1.2%-6.4%. Compared with the results of the traditional spark discharge optical emission spectrometry technique, the analytical performance of LIBS is just a little inferior due to the less stable laser-induced plasma and smaller amount of ablated sample by the laser. However, the precision, detection limits and accuracy of LIBS obtained in our present work were sufficient to meet the requirements for process analysis. These technical performances of higher stability of output energy and longer service life for DPSSL, in comparison to the Q-switch laser pumped by xeon lamp, qualify it well for the real time online analysis for different industrial applications.展开更多
The effect of dew points(-50,-l0 and+10℃)on the galvanizing properties of a high-manganese twinning-inducedplasticity(TWIP)steel was studied.Scanning electron microscopy(SEM),glow discharge optical emission spectrome...The effect of dew points(-50,-l0 and+10℃)on the galvanizing properties of a high-manganese twinning-inducedplasticity(TWIP)steel was studied.Scanning electron microscopy(SEM),glow discharge optical emission spectrometry(GDOES)and X-ray photoelectron spectroscopy(XPS)were used for microscopic observation and qualitative analysis of the interfacial layer between the steel surface and the zinc layer after hot-dip galvanizing.SEM analysis results show thatthree diffcrent morphologies of metallic oxides are formed on the interfacial layer under the different dew points.GDOES results show that Al is present in the molten zinc,reacting with Fe on the steel surface to form Fe2Al5,which can increasethe galvanizing properties.XPS results show that the valence states of Mn in the interfacial alloy layer are Mn'*and Mn*+,and the valence stales of Fe are Fe^0,Fe^2+and Fe^3+.The experimental results show that the hot-dip galvanizing performanceis the best at-10℃ and the formation of Mn and Fe intermetallic oxides has a bad effect on hot-dip galvanizing behaviorof the high-manganese TWIP steel.The types of the formed surface oxides(MnO,Mn3O4,Mn2O3,FeO3,and Fe2MnO4)onthe surface of the steel sheet are confirmed.It can obtain the best hot-dip galvanizing performance of the high-manganese TWIP steel by controlling the dew point from-10 to-5℃.展开更多
基金supported by Standard Substance Research Group,Central Iron and Steel Research Institute
文摘The rapid quantitative analysis of nitrogen in steel with optical emission spectrometry is described.The problems about the selection of spectral line for the determination of nitrogen,the analytical conditions of nitrogen,the preparation of analytical sample,the effect of co-existing element and the calibration curve of nitrogen are discussed.The analytical range of nitrogen is 0.000 5%to 0.30%,the limit of detection is 0.000 374%,the analytical time is less than 2 min(including the preparation of sample and the exciting sample for two times).Nitrogen in steel is simultaneously determined with alloy elements and acid soluble/insoluble compounds of aluminium.
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 Steel Union Foundation of China (No.50374050)
文摘Electron density （Ne） in a glow discharge plasma for the surface alloying technique is diagnosed by optical emission spectrometry （OES）. With CH4 as the feeding gas, Ne is obtained by comparing the Hβ spectrum according to the Stark broadening effect. It is noticed that Ne varies with the working pressures （30 Pa to 70 Pa） and cathode voltages （500 V to 1000 V）, respectively. Due to an abnormal glow discharge, Ne is between 1. 71 × 10^15 /cm^3 to 6.64 × 10^15 /cm^3 and increases rapidly with working gas pressures and cathode voltages. The results show that OES is a useful method to measure the plasma parameters in a surface alloying glow discharge plasma.
基金the National Natural Science Foundation of China(No.21575092)for financial support
文摘An environmentally friendly,low power consuming,sensitive and compact mercury analyzer was developed for the determination of mercury in water samples by integrating a thin film dielectric barrier discharge induced cold vapor reactor and a dielectric barrier discharge optical emission spectrometer into a small polymethyl methacrylate plate（10.5 cm length×8.0 cm width×1.2 cm height）.Mercury cold vapor was generated when standard or sample solutions with or without formic acid were introduced to the reactor to form thin film liquid and exposed to microplasma irradiation and subsequently separated from the liquid phase for transport to the microplasma and detection of its atomic emission.Limits of detection of 0.20 μg L^-1 and 2.6 μg L^-1 were obtained for the proposed system using or not using formic acid,respectively.Compared to the conventional microplasma optical emission spectrometry used for mercury analysis,this system not only retains the good limit of detection amenable to the determination of mercury in real samples,but also reduces power consumption,eliminates the generation of hydrogen and avoids the use of toxic or unstable reductant.Method validation was demonstrated by analysis of a certified reference material of water sample and three real water samples with good spike recoveries（88-102%）.
基金supported by National Natural Science Foundation of China(Grant No.61378037)the Fundamental Research Funds for the Central Universities(Nos.2013B33614,2017B15214)+1 种基金the Research Funds of Innovation and Entrepreneurship Education Reform for Chinese Universities(No.16CCJG01Z004)the Changzhou Science and Technology Program(No.CJ20160027)
文摘The capacitively coupled radio frequency（CCRF）plasma has been widely used in various fields.In some cases,it requires us to estimate the range of key plasma parameters simpler and quicker in order to understand the behavior in plasma.In this paper,a glass vacuum chamber and a pair of plate electrodes were designed and fabricated,using 13.56 MHz radio frequency（RF）discharge technology to ionize the working gas of Ar.This discharge was mathematically described with equivalent circuit model.The discharge voltage and current of the plasma were measured atdifferent pressures and different powers.Based on the capacitively coupled homogeneous discharge model,the equivalent circuit and the analytical formula were established.The plasma density and temperature were calculated by using the equivalent impedance principle and energy balance equation.The experimental results show that when RF discharge power is 50–300 W and pressure is 25–250 Pa,the average electron temperature is about 1.7–2.1 e V and the average electron density is about 0.5？×10^17–3.6？×10^17m^-3.Agreement was found when the results were compared to those given by optical emission spectroscopy and COMSOL simulation.
基金supported by the Development Fund of National Autonomous Demonstration Innovation Zone of Shandong Peninsula(Grant No.ZCQ17104)the National Key Research and Development Program of China(Grant No.2017YFB0305400)‘double hundred plan’ Yantai talent funding project
文摘A diode-pumped solid-state laser （DPSSL） with a high energetic stability and long service life is applied to ablate the steel samples instead of traditional Nd：YAG laser pumped by a xenon lamp, and several factors, such as laser pulse energy, repetition rate and argon flow rate, that influence laser-induced breakdown spectroscopy （LIBS） analytical performance are investigated in detail. Under the optimal experiment conditions, the relative standard deviations for C, Si, Mn, Ni, Cr and Cu are 3.3%-8.9%, 0.9%-2.8%, 1.2%-4.1%, 1.7%-3.0%, 1.1%-3.4% and 2.5%-8.5%, respectively, with the corresponding relative errors of 1.1%-7.9%, 1.0%-6.3%, 0.4%-3.9%, 1.5%-6.3%, 1.2%-4.0% and 1.2%-6.4%. Compared with the results of the traditional spark discharge optical emission spectrometry technique, the analytical performance of LIBS is just a little inferior due to the less stable laser-induced plasma and smaller amount of ablated sample by the laser. However, the precision, detection limits and accuracy of LIBS obtained in our present work were sufficient to meet the requirements for process analysis. These technical performances of higher stability of output energy and longer service life for DPSSL, in comparison to the Q-switch laser pumped by xeon lamp, qualify it well for the real time online analysis for different industrial applications.
基金This work is financially supported by the National Key R&D Program of China(2017YFB0304402)the National Natural Science Foundation of China(51971127).
文摘The effect of dew points(-50,-l0 and+10℃)on the galvanizing properties of a high-manganese twinning-inducedplasticity(TWIP)steel was studied.Scanning electron microscopy(SEM),glow discharge optical emission spectrometry(GDOES)and X-ray photoelectron spectroscopy(XPS)were used for microscopic observation and qualitative analysis of the interfacial layer between the steel surface and the zinc layer after hot-dip galvanizing.SEM analysis results show thatthree diffcrent morphologies of metallic oxides are formed on the interfacial layer under the different dew points.GDOES results show that Al is present in the molten zinc,reacting with Fe on the steel surface to form Fe2Al5,which can increasethe galvanizing properties.XPS results show that the valence states of Mn in the interfacial alloy layer are Mn'*and Mn*+,and the valence stales of Fe are Fe^0,Fe^2+and Fe^3+.The experimental results show that the hot-dip galvanizing performanceis the best at-10℃ and the formation of Mn and Fe intermetallic oxides has a bad effect on hot-dip galvanizing behaviorof the high-manganese TWIP steel.The types of the formed surface oxides(MnO,Mn3O4,Mn2O3,FeO3,and Fe2MnO4)onthe surface of the steel sheet are confirmed.It can obtain the best hot-dip galvanizing performance of the high-manganese TWIP steel by controlling the dew point from-10 to-5℃.
