In public health studies limited volumes of blood are often collected and stored for future hypothesis testing. Archived samples are irreplaceable and therefore it is valuable to develop analytical techniques that req...In public health studies limited volumes of blood are often collected and stored for future hypothesis testing. Archived samples are irreplaceable and therefore it is valuable to develop analytical techniques that require minimal sample vo-lume. This work describes the measurement of trace elements Mg, Cu, Fe, Zn and ultratrace elements Cd, Co, Mn, Pb in limited quantity (150 μL) human serum or plasma samples. Samples were digested using a hotblock and analyzed using inductively coupled plasma mass spectrometry (ICP-MS). The analytical method was evaluated using a quadrupole (Q) and sector field high resolution (SF) instrument to analyze trace elements in Seronorm? quality control serum material. The method was used to analyze 1888 blinded human plasma samples which were archived for the National Cancer Institute from the Nutrition Intervention Trial in Linxian China. The inductively coupled plasma method was capable of accurately analyzed limited quantity samples of human serum and plasma for the trace elements Mg, Cu, Fe Zn and the ultra trace elements Co, Mn and Pb. The concentration of Cd in human plasma samples was below the level of detection for 75% of the samples analyzed.展开更多
A An analytical method using high resolution inductively coupled plasma mass spectrometry (HR-ICP-MS) for rapid simultaneous determination of 24 elements (Be, Mg, A1, Ti, V, Cr, Mn, Fe, Ni, Cu, Zn, Ga, Ge, As, Se, ...A An analytical method using high resolution inductively coupled plasma mass spectrometry (HR-ICP-MS) for rapid simultaneous determination of 24 elements (Be, Mg, A1, Ti, V, Cr, Mn, Fe, Ni, Cu, Zn, Ga, Ge, As, Se, Mo, Ag, Cd, Sn Sb, Ba, Pt, Au, and Pb) in high purity cobalt was described. Sample digestions were performed in closed microwave vessels using HNO3 and HCI. The matrix effects because of the presence of excess HCI and Co were evaluated. The usefulness of high mass resolution for overcoming some spectral interference was demonstrated. The optimum conditions for the determination were tested and discussed. The standard addition method was employed for quantitative analysis. The detection limits were 0.016-1.50 ].tg·g^-1, the recovery ratios were 92.2%-111.2%, and the RSD was less than 3.6%. The method was accurate, quick, and convenient. It was applied to the determination of trace impurities in high purity cobalt with satisfactory results.展开更多
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
An analytical method using high resolution inductively coupled plasma mass spectrometry (HR-ICP-MS) for rapid simultaneous determination of Be, Mg, Al, Ti, V, Cr, Mn, Fe, Ni, Cu, Zn, Ga, Ge, As, Se, Mo, Ag, Cd, Sn, ...An analytical method using high resolution inductively coupled plasma mass spectrometry (HR-ICP-MS) for rapid simultaneous determination of Be, Mg, Al, Ti, V, Cr, Mn, Fe, Ni, Cu, Zn, Ga, Ge, As, Se, Mo, Ag, Cd, Sn, Sb, Ba, Pt, Au and Pb in high purity cobalt was described. Sample digestions were performed in closed microwave vessels using HNO3 and HCl. The matrix effects due to the presence of excess HCl and Co were evaluated. The usefulness of high mass resolution for overcoming some spectral interference was demonstrated. The optimum conditions for the determination was tested and discussed. Correction for matrix effects, Sc, Rh and Bi were used as internal standards. The detection limits is 0.003-0.57 μg/g, the recovery ratio is 92.2%-111.2%, and the RSD is less than 3.6%. The method is accurate, quick and convenient. It has been applied to the determination of trace impurities in high purity cobalt with satisfactory results.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 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
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
Infant rice cereals were analyzed for total arsenic, inorganic arsenic (i-As) and the organic arsenic species monomethylarsonoic acid (MMA) and dimethylarsinic acid (DMA) using liquid chromatography inductively couple...Infant rice cereals were analyzed for total arsenic, inorganic arsenic (i-As) and the organic arsenic species monomethylarsonoic acid (MMA) and dimethylarsinic acid (DMA) using liquid chromatography inductively coupled plasma mass spectrometry (LC-ICP-MS). Total arsenic concentrations in the samples ranged from 110 ng/gup to 420 ng/g. The i-As in the rice cereals accounted for 33% to 77% of the total arsenic. The observed variability between infant rice cereals makes a dietary survey approach to accessing arsenic exposures difficult.展开更多
Trace elements were determined in high purity gold by high resolution inductively coupled plasma mass spectrometry (HR-ICP-MS). Sample were decomposed by aqua regia. To overcome some potentially problematic spectra/...Trace elements were determined in high purity gold by high resolution inductively coupled plasma mass spectrometry (HR-ICP-MS). Sample were decomposed by aqua regia. To overcome some potentially problematic spectra/ interference, measurements were acquired in both medium and high resolution modes. The matrix effects due to the presence of excessive HCl and Au were evaluated. The optimum conditions for the determination was tested and discussed. The standard addition method was employed for quantitative analysis. The detection limits range from 0.01ug/g to 0.28ug/g depending on the elements. The method is accurate, quick and convenient. It has been applied to the determination of trace elements in high purity gold with satisfactory results.展开更多
The contents of Mg,Al,Si,Ti,Cr,Mn,Fe,Co,Cu,Ga,As,Se,Cd,Sb,Pb and Bi in high purity nickel were determined by high resolution inductively coupled plasma mass spectrometry(HR-ICP-MS).The sample was dissolved in HNO3 and...The contents of Mg,Al,Si,Ti,Cr,Mn,Fe,Co,Cu,Ga,As,Se,Cd,Sb,Pb and Bi in high purity nickel were determined by high resolution inductively coupled plasma mass spectrometry(HR-ICP-MS).The sample was dissolved in HNO3 and HCl by microwave digestion.Most of the spectral interferences could be avoided by measuring in the high resolution mode.The matrix effects because of the presence of excess HCl and nickel were evaluated.Correction for matrix effects was made using Sc,Rh and Tl as internal standards.The optimum conditions for the determination were tested and discussed.The detection limits range from 0.012 to 1.76 μg/g depending on the type of elements.The applicability of the proposed method is also validated by the analysis of high purity nickel reference material(NIST SRM 671).The relative standard deviation(RSD) is less than 3.3%.Results for determination of trace elements in high purity nickel were presented.展开更多
In this study, a simple method for the simultaneous determination of trace metals(Cu, V, Co, Zn) in coastal seawater using the Mg(OH)2 coprecipitation inductively coupled plasma mass spectrometry(ICP-MS) was developed...In this study, a simple method for the simultaneous determination of trace metals(Cu, V, Co, Zn) in coastal seawater using the Mg(OH)2 coprecipitation inductively coupled plasma mass spectrometry(ICP-MS) was developed. This multi-element method enables the simultaneous extraction of four metals, particularly Co and V. The recoveries of Cu, Co, V and Zn after Mg(OH)2 coprecipitation were 73%, 96%, 94% and 92%, which means that our procedure was well-suited to the determination of these four trace metals. The detection limits were 3.81, 0.18, 6.09 and 1.91 nmol L-1, respectively. Then, applying this method to the simultaneous determination of these four metals in coastal water samples from the East China Sea revealed that the concentrations of Cu, Zn, Co and V were higher in bottom waters compared to water at other depths, and higher concentrations were generally observed at the Yangtze River estuary. Additionally, example vertical profiles of dissolved trace metal concentrations for the East China Sea in spring and autumn are compared. These findings indicate that Zn had the greatest seasonal variation followed by Cu, V and Co. For Zn and Co, the concentrations were higher during spring than during autumn. For Cu and V, the seasonal variation in the concentrations was opposite.展开更多
The contents of Cr, Cu, Ni, As, Cd and Pb in coal fly ash were determined by a high resolution inductively coupled plasma mass spectrometry method. The sample digestions were performed in closed microwave vessels with...The contents of Cr, Cu, Ni, As, Cd and Pb in coal fly ash were determined by a high resolution inductively coupled plasma mass spectrometry method. The sample digestions were performed in closed microwave vessels with HNO3, HClO4 and HF. The optimum conditions for the determination were obtained. The applicability of the proposed method was validated by the analysis of coal fly ash reference material (NIST SRM 1633a). The results show that most of the spectral interferences can be avoided by measuring in the high resolution mode (maximum mass resolution R=9 000). The detection limit is from 0.05 to 0.21 μg/g, and the precision is fine with relative standard deviation less than 4.3%.展开更多
An inductively coupled plasma mass spectrometry(ICP-MS) method was developed for the determination of Na, Mg, Al,K, Ca, Ti, Cr, Co, Ni, Cu, Ga, As, Mo, Ag, Cd and Pb in MnZn ferrites. The sample was digested by HNO3+H...An inductively coupled plasma mass spectrometry(ICP-MS) method was developed for the determination of Na, Mg, Al,K, Ca, Ti, Cr, Co, Ni, Cu, Ga, As, Mo, Ag, Cd and Pb in MnZn ferrites. The sample was digested by HNO3+HCl with microwave digestion followed by dilution with ultrapure water, then the above 16 impurity elements in the solution were analyzed directly by ICP-MS. The impurity elements were introduced by the helium gas or hydrogen gas into the octopole reaction system(ORS) to eliminate the polyatomic interferences caused by the high salty matrixes. The matrix effect was minimized through matrix matching,and Be, Y and Rh were used as internal standard elements. The working parameters of the instrument were optimized. The results show that the method has good precision and high accuracy. The detection limits for the investigated elements are in the range of0.9-37.5 ng/L, the relative standard deviation of each element is within 1.1%-4.8%, and the recovery of each element is 90%-108%.展开更多
An analytical method, using sector field inductively coupled plasma mass spectrometry(SF-ICP-MS) for rapid simultaneous determination of Be, Na, Mg, Si, Ca, Ti, V, Cr, Fe, Co, Ni, Cu, Zn, As, Sn, Sb, Pb and Bi in elec...An analytical method, using sector field inductively coupled plasma mass spectrometry(SF-ICP-MS) for rapid simultaneous determination of Be, Na, Mg, Si, Ca, Ti, V, Cr, Fe, Co, Ni, Cu, Zn, As, Sn, Sb, Pb and Bi in electrolytic manganese metal, was described. At the beginning, the samples were decomposed by HNO3 and H2 SO4, and then analyzed by SF-ICP-MS. Most of the spectral interferences could be avoided by measuring in different mass resolution modes. The matrix effects due to the excess of sulfuric acid and Mn were evaluated. Correction of matrix effects was conducted by using the internal standard elements. The optimum condition for the determination was investigated and discussed. The detection limit is in the range of 0.001 0.169 μg/L. The current method is applied to the determination of trace impurities in electrolytic manganese metal. And experiments show that good results can be obtained much faster, more accurately and conveniently by current method.展开更多
This study aimed to evaluate the uncertainty of simultaneous determination of lead(Pb),cadmium(Cd)and arsenic(As)in cosmetics by microwave digestion-inductively coupled plasma mass spectrometry(ICP-MS)with ^72Ge,^115I...This study aimed to evaluate the uncertainty of simultaneous determination of lead(Pb),cadmium(Cd)and arsenic(As)in cosmetics by microwave digestion-inductively coupled plasma mass spectrometry(ICP-MS)with ^72Ge,^115In and ^209Bi as internal standards.According to the method of Safety and Technical Standards for Cosmetics(2015),a mathematical model was established to evaluate the sources and components of uncertainty for the determination of lead,cadmium and arsenic in cosmetics.The results showed that the uncertainties in the determination of lead,cadmium,and arsenic elements in cosmetics were(10.1±0.6)mg/kg,k=2,(4.84±0.28)mg/kg,k=2,(2.04±0.18)mg/kg,k=2,respectively.The main factors that affect the uncertainty of determination results were standard substance,calibration curve,recovery and measurement repeatability.展开更多
Gas chromatography/inductively coupled plasma mass spectrometry (GC/ICP-MS) coupled with solid phase micro-extraction can provide a simple, extremely selective and sensitive technique for the analysis of volatile sulf...Gas chromatography/inductively coupled plasma mass spectrometry (GC/ICP-MS) coupled with solid phase micro-extraction can provide a simple, extremely selective and sensitive technique for the analysis of volatile sulfur and selenium compounds in the headspace of growing plants. In this work, the technique was used to evaluate the volatilization of selenium in wild-type and genetically-modified Brassica juncea seedlings. By converting toxic inorganic selenium in the soil to less toxic, volatile organic selenium, B. juncea might be useful in bioremediation of selenium contaminated soil.展开更多
A system is described in which a graphite furnace electrothermal vaporization device is employed for the introduction of microlitre liquid sample into an inductively coupled argon plasma. The technique provides a pico...A system is described in which a graphite furnace electrothermal vaporization device is employed for the introduction of microlitre liquid sample into an inductively coupled argon plasma. The technique provides a picogram detection limit and an adequate precision with a relative standard deviation of 4%. Mechanism of analyte condensation in transport process is explored. As an application, the technique combined with DDTC/CCl4 extraction is used to enrich and determine non- rare earth impurities in highly pure La2O3.展开更多
In inductively coupled plasma mass spectrometry (ICP-MS) analysis, only a few options are available to deal with non-spectroscopic interferences. Considering that diluting the sample is impractical for traces analysis...In inductively coupled plasma mass spectrometry (ICP-MS) analysis, only a few options are available to deal with non-spectroscopic interferences. Considering that diluting the sample is impractical for traces analysis, other alternatives must be employed. Traditionally, the method of standard additions is used to correct the matrix effect but it is a time consuming method. Others methods involves separation techniques. Another way to overcome matrix interferences is to understand the mechanism involved and adjust plasma viewing conditions to reduce or eliminate the effect. In this study, the effect of various concomitant elements in ICP-MS was assessed by measuring the distribution of selected singly charged analyte ions (Al, V, Cr, Mn, Ni, Co, Cu, Zn, As, In, Ba, La, Ce, Pb), doubly charged ions (La, Ce, Ba and Pb) and oxides ions (BaO) in the presence of concomitant elements spanning a mass range from 23 (Na) to 133 (Cs) u.m.a. and different ionization energies. Concomitant elements are alkali metals, alkaline earth metals and Si. Analyte ion suppression was observed while moving the ICP across and away from the sampling interface with or without a single concomitant element. Matrix effect measures were realised, firstly, to highlight the relation between the signal extinction of an analyte and the masse of the concomitant element, and secondly to highlight the relation between the removal of the analyte signal and the first ionization energy of the element of matrix. A dependence upon both the mass of the matrix element and the mass of the analyte was observed. The suppression seems increased with increasing matrix element mass and decreased with increasing analyte mass. The effect of the mass of the matrix element was the more significant of the two factors. If space-charge effects were found to be significant for matrix elements of much lower mass, it seems diffusion also played an active part for heavier matrix elements. Finally, some evidence was found for a shift in ion-atom equilibrium for dications and for energy demand regarding oxides.展开更多
A droplet carrying particle is desolvation, vaporization, ionization, and diffusion in an inductively coupled plasma (ICP) to form a cloud of ions. It then is detected as a mass-spectrum peak of individual particle. T...A droplet carrying particle is desolvation, vaporization, ionization, and diffusion in an inductively coupled plasma (ICP) to form a cloud of ions. It then is detected as a mass-spectrum peak of individual particle. The diameter of the particle is derived from its mass, which is calibrated using the peak area. This is the basic principle of measuring single particles using inductively coupled plasma mass spectrometry (ICP-MS). In this paper, a mathematical model describing single particles in plasma is investigated. This makes it possible to investigate the process and contributing factors of single particles measurement by ICP-MS. A series of processes are investigated, which include increasing the droplet temperature to the boiling point, desolvation of the droplets, increasing the particle temperature to the melting point, the particles are melted from a solid to the liquid, increasing the particle temperature to the boiling point, and particle vaporization. The simulation shows that both the atomic (ion) diffusion in the plasma and the incomplete vaporization of the particles are two important factors that limit the signal intensity of the particle’s mass spectrum. The experiment reveals that ICP-MS is very linear for Ag nanoparticles below 100 nm and SiO2 particles below 1000 nm. Both the simulation and experiment reveal the measurement deviation for large particles and that an increase of sampling depth can extend the diffusion time and cause signal suppression. The model can be used to study the mechanisms of monodispersed droplet or single-particle mass spectrometry, analyze the contributing parameters for single particle measurements by ICP-MS and provide a theoretical base for the optimization of single particle measurements in the practical application, such as nanoparticle devices, magnetic materials, biomedical materials additives and consumer products.展开更多
OBJECTIVE Cerebral ischemia or ischemic stroke is due to insufficient blood supply to the brain,which causes hypoxia or ischemia in some areas.This work aimed to quantify the minerals and heavy metals in Qishiwei Zhen...OBJECTIVE Cerebral ischemia or ischemic stroke is due to insufficient blood supply to the brain,which causes hypoxia or ischemia in some areas.This work aimed to quantify the minerals and heavy metals in Qishiwei Zhenzhu pill in vivo and in vitro,analyze its effect on the types and abundance of intestinal flora,and study its mechanism on inflammation and apoptosis pathways as a treatment for cerebral ischemia.METHODS Microwave digestion and inductively coupled plasma mass spectrometry(ICP-MS)were used to determine the minerals and heavy metals in 10 batches of Qishiwei Zhenzhu pill in vitro.With the use of the middle cerebral artery obstruction(MCAO)model,ICP-MS was applied to determine the content of minerals and heavy metals in hepatic portal vein blood,abdominal aortic blood,brain,liver,kidney,hair,urine and feces at different time periods.On this model,the ileum,cecum,and colon tissues were tested for intestinal pathology,and 16S rRNA was used for sequencing.Species taxonomy,αdiversity,and species microbial composition and structure analysis were also performed.Polymerase chain reaction and Western blotting were employed to determine the mRNA and protein expression of p38 MAPK,caspase-3,IL^(-1)βand TNF-αin the ischemic brain tissues of rats.RESULTS The average content of heavy metals in the 10 batches of Qishiwei Zhenzhu pill samples is in the descending order Hg>Cu>Pb.Significant differences in the metal elements are found among Qishiwei Zhenzhu pill from different manufacturers but not among the different batches of the same manufacturer.An extremely low content of heavy metals are absorbed into the blood or accumulated in the brain,liver,kidney,and other tissues.Stool is the main excretion route of minerals and heavy metals from Qishiwei Zhenzhu pill.This medicine helps repair the intestinal mucosa in MCAO rats.At the phylum level,it can regulate the abundance of Firmicutes and Proteobacteria in the intestinal flora of rats with cerebral ischemia.At the genus level,it can adjust the abundance of Escherichia Shigella.At the species level,it can adjust the abundance of Lactobacillus yoelii and Lactobacillus reuteri.Cluster classification results show that Qishiwei Zhenzhu pill can improve the intestinal flora of rats with cerebral ischemia,reduce the mRNA and protein expression of caspase-3 and IL^(-1)βin rat brain tissues,and have a tendency to decrease the mRNA expression of p38 MAPK and TNF-α.CONCLUSION Quantifying the minerals and heavy metals in Qishiwei Zhenzhu pill in vivo and in vitro will help improve their quality standards.Minerals and heavy metals are mainly excreted in feces,accumulate in extremely low levels in various tissues,and do not damage the intestinal mucosa.The effective material basis of Qishiwei Zhenzhu pill in treating cerebral ischemia may be related to their Li,Cr,and Cd elements.These pills can improve the environment of intestinal flora,and their mechanism of treatment for cerebral ischemia may be related to the down-regulation of IL^(-1)βinflammatory factor and inhibition of cell apoptosis.展开更多
文摘In public health studies limited volumes of blood are often collected and stored for future hypothesis testing. Archived samples are irreplaceable and therefore it is valuable to develop analytical techniques that require minimal sample vo-lume. This work describes the measurement of trace elements Mg, Cu, Fe, Zn and ultratrace elements Cd, Co, Mn, Pb in limited quantity (150 μL) human serum or plasma samples. Samples were digested using a hotblock and analyzed using inductively coupled plasma mass spectrometry (ICP-MS). The analytical method was evaluated using a quadrupole (Q) and sector field high resolution (SF) instrument to analyze trace elements in Seronorm? quality control serum material. The method was used to analyze 1888 blinded human plasma samples which were archived for the National Cancer Institute from the Nutrition Intervention Trial in Linxian China. The inductively coupled plasma method was capable of accurately analyzed limited quantity samples of human serum and plasma for the trace elements Mg, Cu, Fe Zn and the ultra trace elements Co, Mn and Pb. The concentration of Cd in human plasma samples was below the level of detection for 75% of the samples analyzed.
基金the Natural Science Foundation of Hunan Province, China (No. 05JJ40017).
文摘A An analytical method using high resolution inductively coupled plasma mass spectrometry (HR-ICP-MS) for rapid simultaneous determination of 24 elements (Be, Mg, A1, Ti, V, Cr, Mn, Fe, Ni, Cu, Zn, Ga, Ge, As, Se, Mo, Ag, Cd, Sn Sb, Ba, Pt, Au, and Pb) in high purity cobalt was described. Sample digestions were performed in closed microwave vessels using HNO3 and HCI. The matrix effects because of the presence of excess HCI and Co were evaluated. The usefulness of high mass resolution for overcoming some spectral interference was demonstrated. The optimum conditions for the determination were tested and discussed. The standard addition method was employed for quantitative analysis. The detection limits were 0.016-1.50 ].tg·g^-1, the recovery ratios were 92.2%-111.2%, and the RSD was less than 3.6%. The method was accurate, quick, and convenient. It was applied to the determination of trace impurities in high purity cobalt with satisfactory results.
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%.
基金supported by the Natural Science Foundation of Hunan Province(No.05JJ40017)Education Department of Hunan Province(No.05B064).
文摘An analytical method using high resolution inductively coupled plasma mass spectrometry (HR-ICP-MS) for rapid simultaneous determination of Be, Mg, Al, Ti, V, Cr, Mn, Fe, Ni, Cu, Zn, Ga, Ge, As, Se, Mo, Ag, Cd, Sn, Sb, Ba, Pt, Au and Pb in high purity cobalt was described. Sample digestions were performed in closed microwave vessels using HNO3 and HCl. The matrix effects due to the presence of excess HCl and Co were evaluated. The usefulness of high mass resolution for overcoming some spectral interference was demonstrated. The optimum conditions for the determination was tested and discussed. Correction for matrix effects, Sc, Rh and Bi were used as internal standards. The detection limits is 0.003-0.57 μg/g, the recovery ratio is 92.2%-111.2%, and the RSD is less than 3.6%. The method is accurate, quick and convenient. It has been applied to the determination of trace impurities in high purity cobalt with satisfactory results.
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 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.
文摘Infant rice cereals were analyzed for total arsenic, inorganic arsenic (i-As) and the organic arsenic species monomethylarsonoic acid (MMA) and dimethylarsinic acid (DMA) using liquid chromatography inductively coupled plasma mass spectrometry (LC-ICP-MS). Total arsenic concentrations in the samples ranged from 110 ng/gup to 420 ng/g. The i-As in the rice cereals accounted for 33% to 77% of the total arsenic. The observed variability between infant rice cereals makes a dietary survey approach to accessing arsenic exposures difficult.
基金Funded by the Hunan Provincial Natural Science Foundation of China(No.05JJ40017)Hunan Provincial Education Department of China (No.07C029 , 08C260)
文摘Trace elements were determined in high purity gold by high resolution inductively coupled plasma mass spectrometry (HR-ICP-MS). Sample were decomposed by aqua regia. To overcome some potentially problematic spectra/ interference, measurements were acquired in both medium and high resolution modes. The matrix effects due to the presence of excessive HCl and Au were evaluated. The optimum conditions for the determination was tested and discussed. The standard addition method was employed for quantitative analysis. The detection limits range from 0.01ug/g to 0.28ug/g depending on the elements. The method is accurate, quick and convenient. It has been applied to the determination of trace elements in high purity gold with satisfactory results.
基金Project(21075138) supported by the National Natural Science Foundation of ChinaProject(cstc2011jjA0780) supported by Natural Science Foundation of Chongqing City,ChinaProject(KJ121311) supported by Educational Commission of Chongqing City of China
文摘The contents of Mg,Al,Si,Ti,Cr,Mn,Fe,Co,Cu,Ga,As,Se,Cd,Sb,Pb and Bi in high purity nickel were determined by high resolution inductively coupled plasma mass spectrometry(HR-ICP-MS).The sample was dissolved in HNO3 and HCl by microwave digestion.Most of the spectral interferences could be avoided by measuring in the high resolution mode.The matrix effects because of the presence of excess HCl and nickel were evaluated.Correction for matrix effects was made using Sc,Rh and Tl as internal standards.The optimum conditions for the determination were tested and discussed.The detection limits range from 0.012 to 1.76 μg/g depending on the type of elements.The applicability of the proposed method is also validated by the analysis of high purity nickel reference material(NIST SRM 671).The relative standard deviation(RSD) is less than 3.3%.Results for determination of trace elements in high purity nickel were presented.
基金financially supported by the National Natural Science Foundation of China (Nos. 41140037, 41276069)the Young Scientist Award Science Foundation of Shandong, China (BS2010HZ026)the Open Science Funding of the Key Laboratory of the First Institute of Oceanography, SOA (MESE-2011-03)
文摘In this study, a simple method for the simultaneous determination of trace metals(Cu, V, Co, Zn) in coastal seawater using the Mg(OH)2 coprecipitation inductively coupled plasma mass spectrometry(ICP-MS) was developed. This multi-element method enables the simultaneous extraction of four metals, particularly Co and V. The recoveries of Cu, Co, V and Zn after Mg(OH)2 coprecipitation were 73%, 96%, 94% and 92%, which means that our procedure was well-suited to the determination of these four trace metals. The detection limits were 3.81, 0.18, 6.09 and 1.91 nmol L-1, respectively. Then, applying this method to the simultaneous determination of these four metals in coastal water samples from the East China Sea revealed that the concentrations of Cu, Zn, Co and V were higher in bottom waters compared to water at other depths, and higher concentrations were generally observed at the Yangtze River estuary. Additionally, example vertical profiles of dissolved trace metal concentrations for the East China Sea in spring and autumn are compared. These findings indicate that Zn had the greatest seasonal variation followed by Cu, V and Co. For Zn and Co, the concentrations were higher during spring than during autumn. For Cu and V, the seasonal variation in the concentrations was opposite.
基金Project (04JJ40016) supported by the Natural Science Foundation of Hunan Province, China
文摘The contents of Cr, Cu, Ni, As, Cd and Pb in coal fly ash were determined by a high resolution inductively coupled plasma mass spectrometry method. The sample digestions were performed in closed microwave vessels with HNO3, HClO4 and HF. The optimum conditions for the determination were obtained. The applicability of the proposed method was validated by the analysis of coal fly ash reference material (NIST SRM 1633a). The results show that most of the spectral interferences can be avoided by measuring in the high resolution mode (maximum mass resolution R=9 000). The detection limit is from 0.05 to 0.21 μg/g, and the precision is fine with relative standard deviation less than 4.3%.
基金Project(21271187)supported by the National Natural Science Foundation of ChinaProject(cstc2013jcyj A10088)supported by the Chongqing Natural Science Foundation,China+1 种基金Projects(2013FJ3093,2013SK3268)supported by the Science and Technology Project of Hunan Province,ChinaProject(KJZH14217)supported by Achievement Transfer Education in Chongqing,China
文摘An inductively coupled plasma mass spectrometry(ICP-MS) method was developed for the determination of Na, Mg, Al,K, Ca, Ti, Cr, Co, Ni, Cu, Ga, As, Mo, Ag, Cd and Pb in MnZn ferrites. The sample was digested by HNO3+HCl with microwave digestion followed by dilution with ultrapure water, then the above 16 impurity elements in the solution were analyzed directly by ICP-MS. The impurity elements were introduced by the helium gas or hydrogen gas into the octopole reaction system(ORS) to eliminate the polyatomic interferences caused by the high salty matrixes. The matrix effect was minimized through matrix matching,and Be, Y and Rh were used as internal standard elements. The working parameters of the instrument were optimized. The results show that the method has good precision and high accuracy. The detection limits for the investigated elements are in the range of0.9-37.5 ng/L, the relative standard deviation of each element is within 1.1%-4.8%, and the recovery of each element is 90%-108%.
基金Project(21075138)supported by the National Natural Science Foundation of ChinaProject(cstc2013jcyjA10088)supported by Chongqing Natural Science Foundation,ChinaProject(KJ121311)supported by Scientific and Technological Research Program of Chongqing Municipal Education Commission,China
文摘An analytical method, using sector field inductively coupled plasma mass spectrometry(SF-ICP-MS) for rapid simultaneous determination of Be, Na, Mg, Si, Ca, Ti, V, Cr, Fe, Co, Ni, Cu, Zn, As, Sn, Sb, Pb and Bi in electrolytic manganese metal, was described. At the beginning, the samples were decomposed by HNO3 and H2 SO4, and then analyzed by SF-ICP-MS. Most of the spectral interferences could be avoided by measuring in different mass resolution modes. The matrix effects due to the excess of sulfuric acid and Mn were evaluated. Correction of matrix effects was conducted by using the internal standard elements. The optimum condition for the determination was investigated and discussed. The detection limit is in the range of 0.001 0.169 μg/L. The current method is applied to the determination of trace impurities in electrolytic manganese metal. And experiments show that good results can be obtained much faster, more accurately and conveniently by current method.
文摘This study aimed to evaluate the uncertainty of simultaneous determination of lead(Pb),cadmium(Cd)and arsenic(As)in cosmetics by microwave digestion-inductively coupled plasma mass spectrometry(ICP-MS)with ^72Ge,^115In and ^209Bi as internal standards.According to the method of Safety and Technical Standards for Cosmetics(2015),a mathematical model was established to evaluate the sources and components of uncertainty for the determination of lead,cadmium and arsenic in cosmetics.The results showed that the uncertainties in the determination of lead,cadmium,and arsenic elements in cosmetics were(10.1±0.6)mg/kg,k=2,(4.84±0.28)mg/kg,k=2,(2.04±0.18)mg/kg,k=2,respectively.The main factors that affect the uncertainty of determination results were standard substance,calibration curve,recovery and measurement repeatability.
文摘Gas chromatography/inductively coupled plasma mass spectrometry (GC/ICP-MS) coupled with solid phase micro-extraction can provide a simple, extremely selective and sensitive technique for the analysis of volatile sulfur and selenium compounds in the headspace of growing plants. In this work, the technique was used to evaluate the volatilization of selenium in wild-type and genetically-modified Brassica juncea seedlings. By converting toxic inorganic selenium in the soil to less toxic, volatile organic selenium, B. juncea might be useful in bioremediation of selenium contaminated soil.
文摘A system is described in which a graphite furnace electrothermal vaporization device is employed for the introduction of microlitre liquid sample into an inductively coupled argon plasma. The technique provides a picogram detection limit and an adequate precision with a relative standard deviation of 4%. Mechanism of analyte condensation in transport process is explored. As an application, the technique combined with DDTC/CCl4 extraction is used to enrich and determine non- rare earth impurities in highly pure La2O3.
文摘In inductively coupled plasma mass spectrometry (ICP-MS) analysis, only a few options are available to deal with non-spectroscopic interferences. Considering that diluting the sample is impractical for traces analysis, other alternatives must be employed. Traditionally, the method of standard additions is used to correct the matrix effect but it is a time consuming method. Others methods involves separation techniques. Another way to overcome matrix interferences is to understand the mechanism involved and adjust plasma viewing conditions to reduce or eliminate the effect. In this study, the effect of various concomitant elements in ICP-MS was assessed by measuring the distribution of selected singly charged analyte ions (Al, V, Cr, Mn, Ni, Co, Cu, Zn, As, In, Ba, La, Ce, Pb), doubly charged ions (La, Ce, Ba and Pb) and oxides ions (BaO) in the presence of concomitant elements spanning a mass range from 23 (Na) to 133 (Cs) u.m.a. and different ionization energies. Concomitant elements are alkali metals, alkaline earth metals and Si. Analyte ion suppression was observed while moving the ICP across and away from the sampling interface with or without a single concomitant element. Matrix effect measures were realised, firstly, to highlight the relation between the signal extinction of an analyte and the masse of the concomitant element, and secondly to highlight the relation between the removal of the analyte signal and the first ionization energy of the element of matrix. A dependence upon both the mass of the matrix element and the mass of the analyte was observed. The suppression seems increased with increasing matrix element mass and decreased with increasing analyte mass. The effect of the mass of the matrix element was the more significant of the two factors. If space-charge effects were found to be significant for matrix elements of much lower mass, it seems diffusion also played an active part for heavier matrix elements. Finally, some evidence was found for a shift in ion-atom equilibrium for dications and for energy demand regarding oxides.
文摘A droplet carrying particle is desolvation, vaporization, ionization, and diffusion in an inductively coupled plasma (ICP) to form a cloud of ions. It then is detected as a mass-spectrum peak of individual particle. The diameter of the particle is derived from its mass, which is calibrated using the peak area. This is the basic principle of measuring single particles using inductively coupled plasma mass spectrometry (ICP-MS). In this paper, a mathematical model describing single particles in plasma is investigated. This makes it possible to investigate the process and contributing factors of single particles measurement by ICP-MS. A series of processes are investigated, which include increasing the droplet temperature to the boiling point, desolvation of the droplets, increasing the particle temperature to the melting point, the particles are melted from a solid to the liquid, increasing the particle temperature to the boiling point, and particle vaporization. The simulation shows that both the atomic (ion) diffusion in the plasma and the incomplete vaporization of the particles are two important factors that limit the signal intensity of the particle’s mass spectrum. The experiment reveals that ICP-MS is very linear for Ag nanoparticles below 100 nm and SiO2 particles below 1000 nm. Both the simulation and experiment reveal the measurement deviation for large particles and that an increase of sampling depth can extend the diffusion time and cause signal suppression. The model can be used to study the mechanisms of monodispersed droplet or single-particle mass spectrometry, analyze the contributing parameters for single particle measurements by ICP-MS and provide a theoretical base for the optimization of single particle measurements in the practical application, such as nanoparticle devices, magnetic materials, biomedical materials additives and consumer products.
文摘OBJECTIVE Cerebral ischemia or ischemic stroke is due to insufficient blood supply to the brain,which causes hypoxia or ischemia in some areas.This work aimed to quantify the minerals and heavy metals in Qishiwei Zhenzhu pill in vivo and in vitro,analyze its effect on the types and abundance of intestinal flora,and study its mechanism on inflammation and apoptosis pathways as a treatment for cerebral ischemia.METHODS Microwave digestion and inductively coupled plasma mass spectrometry(ICP-MS)were used to determine the minerals and heavy metals in 10 batches of Qishiwei Zhenzhu pill in vitro.With the use of the middle cerebral artery obstruction(MCAO)model,ICP-MS was applied to determine the content of minerals and heavy metals in hepatic portal vein blood,abdominal aortic blood,brain,liver,kidney,hair,urine and feces at different time periods.On this model,the ileum,cecum,and colon tissues were tested for intestinal pathology,and 16S rRNA was used for sequencing.Species taxonomy,αdiversity,and species microbial composition and structure analysis were also performed.Polymerase chain reaction and Western blotting were employed to determine the mRNA and protein expression of p38 MAPK,caspase-3,IL^(-1)βand TNF-αin the ischemic brain tissues of rats.RESULTS The average content of heavy metals in the 10 batches of Qishiwei Zhenzhu pill samples is in the descending order Hg>Cu>Pb.Significant differences in the metal elements are found among Qishiwei Zhenzhu pill from different manufacturers but not among the different batches of the same manufacturer.An extremely low content of heavy metals are absorbed into the blood or accumulated in the brain,liver,kidney,and other tissues.Stool is the main excretion route of minerals and heavy metals from Qishiwei Zhenzhu pill.This medicine helps repair the intestinal mucosa in MCAO rats.At the phylum level,it can regulate the abundance of Firmicutes and Proteobacteria in the intestinal flora of rats with cerebral ischemia.At the genus level,it can adjust the abundance of Escherichia Shigella.At the species level,it can adjust the abundance of Lactobacillus yoelii and Lactobacillus reuteri.Cluster classification results show that Qishiwei Zhenzhu pill can improve the intestinal flora of rats with cerebral ischemia,reduce the mRNA and protein expression of caspase-3 and IL^(-1)βin rat brain tissues,and have a tendency to decrease the mRNA expression of p38 MAPK and TNF-α.CONCLUSION Quantifying the minerals and heavy metals in Qishiwei Zhenzhu pill in vivo and in vitro will help improve their quality standards.Minerals and heavy metals are mainly excreted in feces,accumulate in extremely low levels in various tissues,and do not damage the intestinal mucosa.The effective material basis of Qishiwei Zhenzhu pill in treating cerebral ischemia may be related to their Li,Cr,and Cd elements.These pills can improve the environment of intestinal flora,and their mechanism of treatment for cerebral ischemia may be related to the down-regulation of IL^(-1)βinflammatory factor and inhibition of cell apoptosis.