Using ICP-AES with microwave digestion, we determined the concentrations of 16 trace elements in oysters from six sampling points in Jiaozhou Bay.The distributions of the wholesome elements Zn, Fe and Mn, and heavy me...Using ICP-AES with microwave digestion, we determined the concentrations of 16 trace elements in oysters from six sampling points in Jiaozhou Bay.The distributions of the wholesome elements Zn, Fe and Mn, and heavy metals such as As,Cd,Hg and Pb were studied.The oysters collected are all rich in the wholesome trace elements,and the oysters from Licun River have the highest concentrations of the three wholesome trace elements.The concentrations of heavy metals in oysters from Licun River are the highest and those from Hongdao are the lowest. Compared with the domestic and foreign sea-areas,the heavy metal contents in the oysters from Jiaozhou Bay are less in amount than those from some developed countries, and more than those in Southeast China.This implies that the Jiaozhou Bay's oysters have been polluted by the environment to some extent.展开更多
A closed-vessel microwave digestion method is described for the rapid dissolution of environmental samples such as foods, soils and sediments. Depending on the sample type, 0.1-0.2 g sample was decomposed with HNO3/H2...A closed-vessel microwave digestion method is described for the rapid dissolution of environmental samples such as foods, soils and sediments. Depending on the sample type, 0.1-0.2 g sample was decomposed with HNO3/H2O2 or HNO3 / H2O2/HF acid mixture in a PTFE digestion vessel by using microwave heating for 2-3 min at 500W of microwave power. The solution, or to which 0.5 g of boric acid was added, was diluted to 25-50 ml and directly determined by sequential ICP-AES. The accuracy of the procedure was validated by the analysis of six standard reference materials for 10 elements. Ail results were in a good agreements with the certified values.展开更多
The application of non-suppressed ion chromatography for monitoring of trace elements in air particulate matter was studied in the present investigation. The results indicate that the use of microwave acid digestion m...The application of non-suppressed ion chromatography for monitoring of trace elements in air particulate matter was studied in the present investigation. The results indicate that the use of microwave acid digestion method is superior in comparison with the conventional thermal acid digestion method as it leads to higher recovery, better reproducibility, lower volatility loss, better protection against environmental contamination and much less digestion time (5 minutes vs. 24 hours). The use of eluent as extractant is shown to reduce the water dip problem in the chro-matogram. The addition of chelating agent in the eluent coupled with UV detection is shown to provide satisfactory chromatographic separation and good sensitivity for the analysis of transition metals present in the air particulate matter. Using the U.S. National Bureau of Standards Reference Material 1648 Urban Particulate Matter as standard for checking, the analytical procedure is shown to give good recovery and reproducibility for the detection of the following cations and anions in air particulate matter: Fe2 Cu, Mn, Pb, Zn, Mg, Na, HN4+, Cl-, NO3- and SO42-. Field test was also performed to check the applicability of the method and the results obtained were discussed in the present paper.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
[Objectives] This study was conducted to establish an analytical method for the establishment of 13 trace elements in Anshun thorn pear(Rosa roxburghii) and golden thorn pear(Rosa sterilis S. D. Shi). [Methods] Nitric...[Objectives] This study was conducted to establish an analytical method for the establishment of 13 trace elements in Anshun thorn pear(Rosa roxburghii) and golden thorn pear(Rosa sterilis S. D. Shi). [Methods] Nitric acid was used as the digestion system for microwave digestion. Inductively coupled plasma mass spectrometry(ICP-MS) was used to determine the trace elements in thorn pear and golden thorn pear. [Results] Be, Ti, V, Cr, Mn, Co, Ni, As, Sr, Mo, Cd, Sb and Hg were determined by ICP-MS method in thorn pear and golden thorn pear. The correlation coefficients of the regression equations of the elements were higher than 0.996; the precision RSD was lower than 2.87%; and the recovery ranged from 94.3% to 109.8%. [Conclusions] The method has the advantages of high sensitivity, good accuracy and simultaneous detection of multiple elements, and provides a reference method and theoretical basis for determining trace elements in thorn pear and golden thorn pear and other fruits.展开更多
With the emerging concern on trace element content in rice on both toxicological and nutritional standpoints, validation of analytical method to determine both essential and toxic elements in rice is important in orde...With the emerging concern on trace element content in rice on both toxicological and nutritional standpoints, validation of analytical method to determine both essential and toxic elements in rice is important in order to produce reliable results. Therefore, this study was aimed to validate analytical method to determine As, Cd, Pb, Hg, Cr, Ni, Se, Cu, Mn, Mo, Fe, Co and Zn in rice while giving an overview of the challenges encountered and application of the method to analysis trace elements in selected traditional rice varieties available in Sri Lankan market. Sample digestion was carried out by microwave digestion and analysed by ICP-MS. The analytical method was validated by measuring precision, accuracy, limits of detection (LODs), limits of quantification (LOQs), working and linear range, recovery percentage and measurement uncertainty. They showed that the method is fit for its purpose as those complies with the standard method performance requirements of AOAC. Percentage of relative standard deviations (RSD) of repeatability was not greater than 9.9% and RSDs (%) of reproducibility were not greater than 10.1% for all elements. Mean recoveries varied from 81% to 110%. Limits of detections of elements were in the range of 0.04 - 0.8 mg/kg and LOQs were in the range of 0.05 - 1.2 mg/kg. Expanded uncertainties of trace elements lay between 1.1% and 6.0%. Good agreement with the certified values of Standard Reference Material (SRM) 1568b—Rice Flour analysed by the proposed method with recovery percentages between 89.4% and 105.7% further confirms the accuracy and traceability of the method. The distribution pattern of essential elements in all rice varieties analysed was Mn > Zn > Fe > Cu > Mo > Se > Co. Even though arsenic was detected in all varieties, only the mean concentration of lead of Kaluneenati exceeds the maximum level (FAO/WHO CODEX Alimentarius).展开更多
The determination of trace impurities in high purity zinc oxide by high resolution inductively coupled plasma mass spectrometry ( HR-ICP-MS ) was investigated. To overcome some poteutially problematic spectral iuter...The determination of trace impurities in high purity zinc oxide by high resolution inductively coupled plasma mass spectrometry ( HR-ICP-MS ) was investigated. To overcome some poteutially problematic spectral iuterference, measurements were acquired in both middle and high resolution modes. The matrix effects due to the presence of excess HCl and zinc were evaluated. The optimum conditions for the determination were tested and discussed. The standard addition method was employed for quantitative analysis. The detection limits ranged from 0.02μg/ g to 6 μg/ g depending on the elements. The experimental resalts for the determination of Na, Mg, Ca, Cr, Mn, Fe, Co, Ni, Cu, Mo, Cd, Sb and Pb in several high purity zinc oxide powders were presented.展开更多
基金the financial support for thisproject by the National Natural Science Foundation ofChina(No.21071133)
文摘Using ICP-AES with microwave digestion, we determined the concentrations of 16 trace elements in oysters from six sampling points in Jiaozhou Bay.The distributions of the wholesome elements Zn, Fe and Mn, and heavy metals such as As,Cd,Hg and Pb were studied.The oysters collected are all rich in the wholesome trace elements,and the oysters from Licun River have the highest concentrations of the three wholesome trace elements.The concentrations of heavy metals in oysters from Licun River are the highest and those from Hongdao are the lowest. Compared with the domestic and foreign sea-areas,the heavy metal contents in the oysters from Jiaozhou Bay are less in amount than those from some developed countries, and more than those in Southeast China.This implies that the Jiaozhou Bay's oysters have been polluted by the environment to some extent.
文摘A closed-vessel microwave digestion method is described for the rapid dissolution of environmental samples such as foods, soils and sediments. Depending on the sample type, 0.1-0.2 g sample was decomposed with HNO3/H2O2 or HNO3 / H2O2/HF acid mixture in a PTFE digestion vessel by using microwave heating for 2-3 min at 500W of microwave power. The solution, or to which 0.5 g of boric acid was added, was diluted to 25-50 ml and directly determined by sequential ICP-AES. The accuracy of the procedure was validated by the analysis of six standard reference materials for 10 elements. Ail results were in a good agreements with the certified values.
文摘The application of non-suppressed ion chromatography for monitoring of trace elements in air particulate matter was studied in the present investigation. The results indicate that the use of microwave acid digestion method is superior in comparison with the conventional thermal acid digestion method as it leads to higher recovery, better reproducibility, lower volatility loss, better protection against environmental contamination and much less digestion time (5 minutes vs. 24 hours). The use of eluent as extractant is shown to reduce the water dip problem in the chro-matogram. The addition of chelating agent in the eluent coupled with UV detection is shown to provide satisfactory chromatographic separation and good sensitivity for the analysis of transition metals present in the air particulate matter. Using the U.S. National Bureau of Standards Reference Material 1648 Urban Particulate Matter as standard for checking, the analytical procedure is shown to give good recovery and reproducibility for the detection of the following cations and anions in air particulate matter: Fe2 Cu, Mn, Pb, Zn, Mg, Na, HN4+, Cl-, NO3- and SO42-. Field test was also performed to check the applicability of the method and the results obtained were discussed in the present paper.
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 Anshun Science and Technology Innovation Platform Construction Project(ASKP[2017]03)
文摘[Objectives] This study was conducted to establish an analytical method for the establishment of 13 trace elements in Anshun thorn pear(Rosa roxburghii) and golden thorn pear(Rosa sterilis S. D. Shi). [Methods] Nitric acid was used as the digestion system for microwave digestion. Inductively coupled plasma mass spectrometry(ICP-MS) was used to determine the trace elements in thorn pear and golden thorn pear. [Results] Be, Ti, V, Cr, Mn, Co, Ni, As, Sr, Mo, Cd, Sb and Hg were determined by ICP-MS method in thorn pear and golden thorn pear. The correlation coefficients of the regression equations of the elements were higher than 0.996; the precision RSD was lower than 2.87%; and the recovery ranged from 94.3% to 109.8%. [Conclusions] The method has the advantages of high sensitivity, good accuracy and simultaneous detection of multiple elements, and provides a reference method and theoretical basis for determining trace elements in thorn pear and golden thorn pear and other fruits.
文摘With the emerging concern on trace element content in rice on both toxicological and nutritional standpoints, validation of analytical method to determine both essential and toxic elements in rice is important in order to produce reliable results. Therefore, this study was aimed to validate analytical method to determine As, Cd, Pb, Hg, Cr, Ni, Se, Cu, Mn, Mo, Fe, Co and Zn in rice while giving an overview of the challenges encountered and application of the method to analysis trace elements in selected traditional rice varieties available in Sri Lankan market. Sample digestion was carried out by microwave digestion and analysed by ICP-MS. The analytical method was validated by measuring precision, accuracy, limits of detection (LODs), limits of quantification (LOQs), working and linear range, recovery percentage and measurement uncertainty. They showed that the method is fit for its purpose as those complies with the standard method performance requirements of AOAC. Percentage of relative standard deviations (RSD) of repeatability was not greater than 9.9% and RSDs (%) of reproducibility were not greater than 10.1% for all elements. Mean recoveries varied from 81% to 110%. Limits of detections of elements were in the range of 0.04 - 0.8 mg/kg and LOQs were in the range of 0.05 - 1.2 mg/kg. Expanded uncertainties of trace elements lay between 1.1% and 6.0%. Good agreement with the certified values of Standard Reference Material (SRM) 1568b—Rice Flour analysed by the proposed method with recovery percentages between 89.4% and 105.7% further confirms the accuracy and traceability of the method. The distribution pattern of essential elements in all rice varieties analysed was Mn > Zn > Fe > Cu > Mo > Se > Co. Even though arsenic was detected in all varieties, only the mean concentration of lead of Kaluneenati exceeds the maximum level (FAO/WHO CODEX Alimentarius).
文摘The determination of trace impurities in high purity zinc oxide by high resolution inductively coupled plasma mass spectrometry ( HR-ICP-MS ) was investigated. To overcome some poteutially problematic spectral iuterference, measurements were acquired in both middle and high resolution modes. The matrix effects due to the presence of excess HCl and zinc were evaluated. The optimum conditions for the determination were tested and discussed. The standard addition method was employed for quantitative analysis. The detection limits ranged from 0.02μg/ g to 6 μg/ g depending on the elements. The experimental resalts for the determination of Na, Mg, Ca, Cr, Mn, Fe, Co, Ni, Cu, Mo, Cd, Sb and Pb in several high purity zinc oxide powders were presented.