A method based on the combination of coprecipitation with inductively coupledplasma atomic emission spectrometry (ICP-AES) was developed for the determination of impurities inhigh-purity sodium tungstate. Six elements...A method based on the combination of coprecipitation with inductively coupledplasma atomic emission spectrometry (ICP-AES) was developed for the determination of impurities inhigh-purity sodium tungstate. Six elements (Co, Cu, Fe, Mn, Ni, and Pb) were coprecipitated bylanthanum hydroxide so as to be concentrated and separated from the tungsten matrix. Effects of somefactors on the recoveries of the analytes and on the residual amount of sodium tungstate wereinvestigated, and the optimum conditions for the coprecipitation were proposed. Matrix-matchingcalibration curve method was used for the analysis. It is shown that the elements mentioned abovecan be quantitatively recovered. The detection limits for Co, Cu, Fe, Mn, Ni, and Pb are 0.07, 0.4,0.2, 0.1, 0.6, and 1.3 μg·g^(-1), respectively. The recoveries vary from 92.5% to 108%, and therelative standard deviations (RSDs) are in the range of 3.1%-5.5%.展开更多
In the determination of trace yttrium (Y) in an ytterbium (Yb) matrix byinductively coupled plasma atomic emission spectrometry (ICP-AES), the most prominent line ofyttrium, Y 371.030 nm line, suffers from strong inte...In the determination of trace yttrium (Y) in an ytterbium (Yb) matrix byinductively coupled plasma atomic emission spectrometry (ICP-AES), the most prominent line ofyttrium, Y 371.030 nm line, suffers from strong interference due to an emission line of ytterbium.In mis work, a method based on wavelet transform was proposed for the spectral interferencecorrection. Haar wavelet was selected as the mother wavelet. The discrete detail after the thirddecomposition, D3, was chosen for quantitative analysis based on the consideration of bothseparation degree and peak height. The linear correlation coefficient between the height of the leftpositive peak in D3 and the concentration of Y was calculated to be 0.9926. Six synthetic sampleswere analyzed, and the recovery for yttrium varied from 96.3 percent to 110.0 percent. The amountsof yttrium in three ytterbium metal samples were determined by the proposed approach with an averagerelative standard deviation (RSD) of 2.5 percent, and the detection limit for yttrium was 0.016percent. This novel correction technique is fast and convenient, since neither complicated modelassumption nor time-consuming iteration is required. Furthermore, it is not affected by thewavelength drift inherent in monochromators that will severely reduce the accuracy of resultsobtained by some chemometric methods.展开更多
A Kalman filter was developed for correction of wing interference in ICP-AES.Modeling wing interference theoretically instead of experimentally, the filter can compensate the shift in wavelength position in scans, and...A Kalman filter was developed for correction of wing interference in ICP-AES.Modeling wing interference theoretically instead of experimentally, the filter can compensate the shift in wavelength position in scans, and therefore reduce the effect of the interference on detection limit.展开更多
The development of laser sampling for optical emission spectrometry is reviewed . Advantages and limitations of pulsed laser sampling are compared with those of continuous laser sampling . A novel method of laser samp...The development of laser sampling for optical emission spectrometry is reviewed . Advantages and limitations of pulsed laser sampling are compared with those of continuous laser sampling . A novel method of laser sampling of liquid samples for inductively coupled plasma -atomic emission spectrometry has been proposed , and its analytical performance investigated.Experimental results showed that,as a method of sample introduction , laser vaporization of liquid samples enjoyed certain advantages , e.g.,much higher sensitivity, much lower detection limit and reduced sample volume , over solution nebulization . A perspective of the application of laser sampling-inductively coupled plasma - actomic emission spectrometry for rock and mineral analysis is estimated as well.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
In general, atomic emission spectrometry (AES) is an excellent technique for determination of metal elements. However, its capability of determining nonmetals has not been developed well. The major reasons are the res...In general, atomic emission spectrometry (AES) is an excellent technique for determination of metal elements. However, its capability of determining nonmetals has not been developed well. The major reasons are the resonance lines of most nonmetals lie in the vacuum ultraviolet spectral region and the ionic lines of these elements are difficult to be used because the ionization potentials of the elements are very high. And furthermore only He plasma can efficiently excit those ionic resonance lines. The practical application of HeICP-AES to determining the nonmetals is also difficult because its operating and perchace costs are very high. In contrast to HeICPAES, the costs of He microwave induced plasma (MIP)-AES are relatively low, HeMIP has a high excitation capability which can excite ionic lines of various nonmetals and the nonmetals can be determined by HeMIP-AES with a high sensitivity.展开更多
The determination of carbon by means of microwave plasma torch atomic emission spectrometry(MPT-AES) was studied. Aqueous samples were introduced with a pneumatic nebulization system. The detection limit for carbon wa...The determination of carbon by means of microwave plasma torch atomic emission spectrometry(MPT-AES) was studied. Aqueous samples were introduced with a pneumatic nebulization system. The detection limit for carbon was 0. 047μg/mL.The method was applied to the analysis for tap water and results were satisfactory.展开更多
Although the flow injection(FI) as a sample introduction technique has been extensively applied to atomic spectrometry, such as ICP-AES and AAS, very little has been done so far on coupling FI to microwave plasma syst...Although the flow injection(FI) as a sample introduction technique has been extensively applied to atomic spectrometry, such as ICP-AES and AAS, very little has been done so far on coupling FI to microwave plasma systems. Gehlausen et al. determined aqueous fluorine by coupling flow injection analysis (FIA) with HeMIP展开更多
文摘A method based on the combination of coprecipitation with inductively coupledplasma atomic emission spectrometry (ICP-AES) was developed for the determination of impurities inhigh-purity sodium tungstate. Six elements (Co, Cu, Fe, Mn, Ni, and Pb) were coprecipitated bylanthanum hydroxide so as to be concentrated and separated from the tungsten matrix. Effects of somefactors on the recoveries of the analytes and on the residual amount of sodium tungstate wereinvestigated, and the optimum conditions for the coprecipitation were proposed. Matrix-matchingcalibration curve method was used for the analysis. It is shown that the elements mentioned abovecan be quantitatively recovered. The detection limits for Co, Cu, Fe, Mn, Ni, and Pb are 0.07, 0.4,0.2, 0.1, 0.6, and 1.3 μg·g^(-1), respectively. The recoveries vary from 92.5% to 108%, and therelative standard deviations (RSDs) are in the range of 3.1%-5.5%.
文摘In the determination of trace yttrium (Y) in an ytterbium (Yb) matrix byinductively coupled plasma atomic emission spectrometry (ICP-AES), the most prominent line ofyttrium, Y 371.030 nm line, suffers from strong interference due to an emission line of ytterbium.In mis work, a method based on wavelet transform was proposed for the spectral interferencecorrection. Haar wavelet was selected as the mother wavelet. The discrete detail after the thirddecomposition, D3, was chosen for quantitative analysis based on the consideration of bothseparation degree and peak height. The linear correlation coefficient between the height of the leftpositive peak in D3 and the concentration of Y was calculated to be 0.9926. Six synthetic sampleswere analyzed, and the recovery for yttrium varied from 96.3 percent to 110.0 percent. The amountsof yttrium in three ytterbium metal samples were determined by the proposed approach with an averagerelative standard deviation (RSD) of 2.5 percent, and the detection limit for yttrium was 0.016percent. This novel correction technique is fast and convenient, since neither complicated modelassumption nor time-consuming iteration is required. Furthermore, it is not affected by thewavelength drift inherent in monochromators that will severely reduce the accuracy of resultsobtained by some chemometric methods.
文摘A Kalman filter was developed for correction of wing interference in ICP-AES.Modeling wing interference theoretically instead of experimentally, the filter can compensate the shift in wavelength position in scans, and therefore reduce the effect of the interference on detection limit.
文摘The development of laser sampling for optical emission spectrometry is reviewed . Advantages and limitations of pulsed laser sampling are compared with those of continuous laser sampling . A novel method of laser sampling of liquid samples for inductively coupled plasma -atomic emission spectrometry has been proposed , and its analytical performance investigated.Experimental results showed that,as a method of sample introduction , laser vaporization of liquid samples enjoyed certain advantages , e.g.,much higher sensitivity, much lower detection limit and reduced sample volume , over solution nebulization . A perspective of the application of laser sampling-inductively coupled plasma - actomic emission spectrometry for rock and mineral analysis is estimated as well.
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.
文摘In general, atomic emission spectrometry (AES) is an excellent technique for determination of metal elements. However, its capability of determining nonmetals has not been developed well. The major reasons are the resonance lines of most nonmetals lie in the vacuum ultraviolet spectral region and the ionic lines of these elements are difficult to be used because the ionization potentials of the elements are very high. And furthermore only He plasma can efficiently excit those ionic resonance lines. The practical application of HeICP-AES to determining the nonmetals is also difficult because its operating and perchace costs are very high. In contrast to HeICPAES, the costs of He microwave induced plasma (MIP)-AES are relatively low, HeMIP has a high excitation capability which can excite ionic lines of various nonmetals and the nonmetals can be determined by HeMIP-AES with a high sensitivity.
文摘The determination of carbon by means of microwave plasma torch atomic emission spectrometry(MPT-AES) was studied. Aqueous samples were introduced with a pneumatic nebulization system. The detection limit for carbon was 0. 047μg/mL.The method was applied to the analysis for tap water and results were satisfactory.
基金Supported by the National Natural Science Founddation of China
文摘Although the flow injection(FI) as a sample introduction technique has been extensively applied to atomic spectrometry, such as ICP-AES and AAS, very little has been done so far on coupling FI to microwave plasma systems. Gehlausen et al. determined aqueous fluorine by coupling flow injection analysis (FIA) with HeMIP
