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1.
Multielemental instrumental neutron activation (INAA), inductively coupled plasmaatomic emission spectrometric (ICP-AES) and atomic absorption spectrophotometric (AAS) analyses are utilized for the determination of Ag, Al, As, Au, Ba, Be, Br, Ca, Cd, Ce, Cl, Co, Cr, Cu, Eu, Fe, Ga, Hf, K, La, Li, Lu, Mg, Mn, Na, Nb, Ni, P. Pb, Sb, Sc, Se, Sm, Sn, Sr, Ta, Th, Ti, U, V, W and Zn in sugar cane plant, raw juice, juice in different stages, syrup, deposits, molasses, A, B and C sugar, refinery 1 and 2 sugar, and in soil samples picked up from the immediate vicinity of the cane plant roots at surface, 30 and 60 cm depth.  相似文献   

2.
Instrumental neutron activation analysis was used for the determination of Al, Br, Ca, Ce, Cl, Co, Cr, Cs, Eu, Fe, K, La, Mg, Mn, Na, Rb, Sb, Sc, Se, Ti, Th, V and Zn, ICP-AES for the determination Al, Ag, Ba, Be, Ca, Co, Cr, Cu, Fe, Ga, K, Li, Mg, Mn, Na, Ni, P, Sc, Sr, Ti, V and Zn and flameless AAS for the determination of Cd, Hg and Pb in egg plant, potatoes, green pepper (Leguminosae), vegetable marrow (Cucurbitaceae), pears, apple (Rosaceae), castor oil plant (Euphorbiaceae), lettuce (compositae), dill, parsley, coriander (Umbelliferae), and in some soil samples collected from Aswan province.  相似文献   

3.
In order to evaluate alternative analytical methodologies to study the geographical origin of ciders, both multi-elemental analysis and Sr isotope abundance ratios in combination with multivariate statistical analysis were estimated in 67 samples from England, Switzerland, France and two Spanish regions (Asturias and the Basque Country). A methodology for the precise and accurate determination of the 87Sr/86Sr isotope abundance ratio in ciders by multicollector inductively coupled plasma mass spectrometry (MC-ICP-MS) was developed. Major elements (Na, K, Ca and Mg) were measured by ICP-AES and minor and trace elements (Li, Be, B, Al, Sc, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ga, As, Se, Rb, Sr, Y, Mo, Cd, Sn, Sb, Cs, Ba, La, Ce, W, Tl, Pb, Bi, Th and U) were measured by ICP-MS using a collision cell instrument operated in multitune mode. An analysis of variance (ANOVA test) indicated that group means for B, Cr, Fe, Ni, Cu, Se, Cd, Cs, Ce, W, Pb, Bi and U did not show any significant differences at the 95% confidence level, so these elements were rejected for further statistical analysis. Another group of elements (Li, Be, Sc, Co, Ga, Y, Sn, Sb, La, Tl, Th) was removed from the data set because concentrations were close to the limits of detection for many samples. Therefore, the remaining elements (Na, Mg, Al, K, Ca, Ti, V, Mn, Zn, As, Rb, Sr, Mo, Ba) together with 87Sr/86Sr isotope abundance ratio were considered for principal component analysis (PCA) and linear discriminant analysis (LDA). Finally, LDA was able to classify correctly 100% of cider samples coming from different Spanish regions, France, England and Switzerland when considering Na, Mg, Al, K, Ca, Ti, V, Mn, Zn, As, Rb, Sr, Mo, Ba and 87Sr/86Sr isotope abundance ratio as original variables.  相似文献   

4.
A method has been developed for the determination of 23 elements in marine plankton in which inductively coupled plasma (ICP) source mass spectrometry (MS) was used to quantify the elements in the solution after digestion in a mixture of hydrofluoric and nitric acids in sealed PTFE vessels in a microwave field. The procedure was validated by the analysis of a standard reference soil (SRM 2709 San Joaquin Soil) and a standard reference fresh water plankton (CRM 414). The method was applied to the analysis of several marine plankton samples grown under controlled conditions including several whose growth media had been enriched with selenium. Matrix induced signal suppressions and instrumental drift were corrected by internal standardization. The suitabilities of germanium, indium, rhodium, scandium and yttrium as internal standard elements were evaluated. Neither scandium nor yttrium could be used due to the presence of these elements in the samples, germanium was used for the determination of As, Co, Cu, Fe, Ni, Se, Si and Zn, indium was used for Al, Ba, Ca, Eu, Sr, and Tl, and rhodium was used for Cd, Cr, Hg, Mg, Pb, Sb, Sn, and V. For Al, Ca, Cr, Cu, Fe, Mg, Mn, Ni, Si, Sr, V, and Zn internal standardization did not completely compensate for the suppressive effect of the heavier elements and the solutions were diluted. However, for As, Ba, Cd, Co, Eu, Hg, Pb, Sb, Se, Sn and T1, it was possible to obtain accurate results despite the 35-40% suppression in the signals. Isobaric overlap was only a problem in the cases of 42Ca and 78Se; 44Ca and 77Se, respectively, were used. Memory effects were only observed with Hg for which a nitric acid-sodium chloride solution was the most effective wash-out solution. The marine plankton samples were able to tolerate a higher concentration of Hg as the selenium concentration increased.  相似文献   

5.
Microwave-acid digestion (MW-AD) followed by inductively coupled plasma-atomic emission spectrometry (ICP-AES), graphite furnace atomic absorption spectrometry (GFAAS), and hydride generation atomic absorption spectrometry (HGAAS) were examined for the determination of various elements in coal and coal fly ash (CFA). Eight certified reference materials (four coal samples and four CFA samples) were tested. The 10 elements (As, Be, Cd, Co, Cr, Mn, Ni, Pb, Sb, and Se), which are described in the Clean Air Act Amendments (CAAA), were especially considered. For coal, the HF-free MW-AD followed by ICP-AES was successful in the determination of various elements except for As, Be, Cd, Sb, and Se. These elements (except for Sb) were well-determined by use of GFAAS (Be and Cd) and HGAAS (As and Se). For CFA, the addition of HF in the digestion acid mixture was needed for the determination of elements, except for As, Sb, and Se, for which the HF-free MW-AD was applicable. The use of GFAAS (Be and Cd) or HGAAS (Sb and Se) resulted in the successful determination of the elements for which ICP-AES did not work well. The protocol for the determination of the 10 elements in coal and CFA by MW-AD followed by the joint-use of ICP-AES, GFAAS, and HGAAS was established.  相似文献   

6.
A method has been developed for the determination of 23 elements in marine plankton in which inductively coupled plasma (ICP) source mass spectrometry (MS) was used to quantify the elements in the solution after digestion in a mixture of hydrofluoric and nitric acids in sealed PTFE vessels in a microwave field. The procedure was validated by the analysis of a standard reference soil (SRM 2709 San Joaquin Soil) and a standard reference fresh water plankton (CRM 414). The method was applied to the analysis of several marine plankton samples grown under controlled conditions including several whose growth media had been enriched with selenium. Matrix induced signal suppressions and instrumental drift were corrected by internal standardization. The suitabilities of germanium, indium, rhodium, scandium and yttrium as internal standard elements were evaluated. Neither scandium nor yttrium could be used due to the presence of these elements in the samples, germanium was used for the determination of As, Co, Cu, Fe, Ni, Se, Si and Zn, indium was used for Al, Ba, Ca, Eu, Sr, and Tl, and rhodium was used for Cd, Cr, Hg, Mg, Pb, Sb, Sn, and V. For Al, Ca, Cr, Cu, Fe, Mg, Mn, Ni, Si, Sr, V, and Zn internal standardization did not completely compensate for the suppressive effect of the heavier elements and the solutions were diluted. However, for As, Ba, Cd, Co, Eu, Hg, Pb, Sb, Se, Sn and Tl, it was possible to obtain accurate results despite the 35–¶40% suppression in the signals. Isobaric overlap was only a problem in the cases of 42Ca and 78Se; 44Ca and 77Se, respectively, were used. Memory effects were only observed with Hg for which a nitric acid-sodium chloride solution was the most effective wash-out solution. The marine plankton samples were able to tolerate a higher concentration of Hg as the selenium concentration increased.  相似文献   

7.
Summary Multi-element analysis by ICP source mass spectrometry for practically matrix-free natural waters, coming from a granitic area and, therefore, rich in trace elements, has been compared with ICP-atomic emission, ICP atomic fluorescence and atomic absorption spectrometry. The following elements have been investigated and their concentrations are in the decreasing order: Ca, Si, Na, Mg, K, Al; Sr, Mn, Ba, Fe, Rb, Zn, B, U, Y, Li, La, Be, Cs, Co, Cr, V, Sb, Bi, Th, Cu, Cd, Ni, Se, Pb, As, Hg, Mo, Tl, Sn. The concentration ranges were between 10 ppm and <0.01 ppb.As a measure of agreement between the different methods under investigation, two criteria have been used (a) the relative variation coefficient VK (%) of the mean element concentration of an element, determined by different methods in all the 98 water samples and (b) the linear, logarithmic and Spearman rank correlation coefficients between ICP-MS and each of the other methods. Detection limits are given from literature for about 32 elements using different methods.The elements Ca, Na, Mg, K, Mn, Sr, Zn, Fe, Li, Cu have been determined with ICP-MS, ICP-AES and AAS; Al, Ba with ICP-MS and ICP-AES; Si only with ICP-AES, whereas B, Be, Bi, Co, Cr, Cs, Hg, La, Mo, Ni, Pb, Rb, Sb, Sn, Th, Tl, U, V, Y only with ICP-MS. In all 34 of the investigated 36 elements could be analysed by ICP-MS, 14 (from about 20 possible) by AAS, 13 by ICP-AES and 12 by ICP-AFS.The agreement between ICP-MS and ICP-AES as well as between ICP-MS and AAS in most cases is remarkably good according to (a). VK (%) for each element in 98 water samples is in the range from ±2.6 to 10% for Na, Mg, Ca, K, Fe, Sr, Ba, Cu, Li (increasing order). Cd and Zn have unexpectedly higher values (±17.3 and ±20.5%); Cd concentrations are, however, near the detection limit.Comparing the different methods on the basis of correlation coefficients according to (b), gives for the Spearman rank correlation coefficient over the whole range of concentrations, respectively for ICP-MS/ICP-AES, AAS, ICP-AFS in case of Ca: 0.998; 0.984; 0.899; Na: 0.993; 0.991; 0.978; Mg: 0.997; 0.993; 0.959; K: 0.986; 0.942; 0.677; Al: 0.987; -; -; Fe: 0.864; 0.974; 0.701; Mn: 0.989; 0.990; 0.198; Sr: 0.988; 0.992; -; Zn: 0.894; 0.819; 0.300; Cu: -; 0.977; 0.202; Li: -; 0.907; 0.586.It is evident from these trace element concentrations as well as the electrical conductivities, that only about three fourths of the investigated samples are typical granitic waters and the remaining ones are associated with different geological background. The samples have been mainly radon waters with more than 18 nCi/l of Rn-222.
Vergleichende Instrumentelle Multielementanalyse I: Vergleich von ICP-Massenspektrometrie mit ICP-Atomemissionsspektrometrie, ICP-Atomfluorescenzspektrometrie und Atomabsorptionsspektrometrie zur Analyse natürlicher Wässer aus einem Granitgebiet

6th Contribution to the principles of trace analysis of elements and radionuclides

Dedicated to Professor Dr. H. Kelker, Frankfurt, on the occasion of his 65th birthday  相似文献   

8.
Using PIXE (proton induced X-ray emission), PIGE (proton induced gamma emission) and ICP-AES (inductively coupled plasma-atomic emission spectroscopy) the concentrations of the 24 elements Al, As, Ba, Br, Ca, Cl, Co, Cr, Cu, Fe, K, Mg, Mn, Na, Pb, Rb, S, Sb, Si, Sn, Sr, Ti, Zn and Zr in 53 archaeological glass samples from South-Eastern Bulgaria, were determined. The glasses are dated from the 1st to 6th century AD. The analytical data showed the samples to be typical soda-lime-silica glass, with natron as flux. A rather broad range of aluminium, titanium and iron impurities was found, with a tendency for more impure glass in the later periods. The decolouring agents were antimony and manganese oxides, with Sb prevailing in earlier, and Mn in later glass.  相似文献   

9.
An ICP-MS method for determination of 60 elements in plant samples is proposed based on optimization of digestion, recommending use of HF besides HNO3 and H2O2 and calibration procedures, using CRMs for construction of calibration curves. Adequate choice of analytical isotopes and various measurement conditions (cold plasma for the determination of Al, Ba, Ca, Fe, K, Mg, Mn, Na, Si and Sr and DRC mode for determination of Ag, As, Ni, Pd, Pt, Se and V) as well as introduction of appropriate corrections lead to determination of as large number of elements with quadropole ICP-MS as with the more expensive SF-ICP-MS. Two measurements are performed: cold plasma and standard/DRC mode. The analytical characteristics of the method are demonstrated by analysis of five CRMs and the agreement of the experimental results with the certified/information/literature values is very good. Detection limits are low enough to permit the determination of all elements but platinum metals at background level. The applicability of the method is demonstrated by analysis of Taraxacum officinale (dandelion) samples collected from regions with different anthropogenic influence. The results indicate high degree of pollution round the Pb-Zn smelter with As, Cd, Cu, Ni, Pb and Zn and increased concentrations of B, Be, Bi, Hg, In, Mn, Sb, Se, Sn, Ti, Tl, V and Zr. The dandelion sample, collected along a highway has increased concentrations of traffic released elements: Pt, Pd, Rh, Ce, La, Pb as well as Cu, Zn, Ba and Rb.  相似文献   

10.
金属饰品样品用硝酸(20+80)溶液浸泡过夜,采用电感耦合等离子体原子发射光谱法测定金属饰品中铅、镉、铬、汞、锑、砷、硒、钡和镍的溶出量。选择波长为216.9,228.8,267.7,194.2,206.8,189.0,196.0,455.4,216.6nm的9条谱线依次作为测定铅、镉、铬、汞、锑、砷、硒、钡和镍的分析线。铅、镉、铬、锑、砷、硒、钡和镍的质量浓度与其发射强度在10.0mg·L-1以内、汞在2.0mg·L-1以内呈线性关系,检出限(3s)在0.002~0.05mg·L-1之间。方法用于金属饰品的分析,回收率在95.4%~103.0%之间,测定值的相对标准偏差(n=11)在0.68%~2.0%之间。  相似文献   

11.
The relationship between real total contents of the major elements Na, Mg, Al, Si, P, S, K, Ca, Ti, Fe and the trace elements Ag, As, B, Ba, Co, Cr, Cu, Mn, Mo, Ni, Pb, Sb, Se, Sn, V, U, Zn in topsoil from the central part of Vilnius is analysed. The amounts of most elements were determined by energy-dispersive X-ray fluorescence, while amounts of Ag, B, Co were measured by optical atomic emission spectrophotometry. Two factors were distinguished according to major elements: anthropogenic (A) including Ca, Mg, Fe, P, S and clayey (C) including K, Al, Ti. Boron, Mn, Cr and U are significantly correlated with members of both factors, Sb with none of them and other trace elements either with all (Cu, Zn, Pb, Se, Ba, Ni, Co) or with separate (V, Ag, Sn, Mo, As) members of the A-factor. Only B, Mn, Cr, U (partly their additive index Z1) are influenced by the C-factor, while twelve other trace elements (also their additive index Z2) are influenced by the A-factor. The additive index Z of all 17 elements is also affected by the A-factor. Four groups of sites have been distinguished according to normal or higher contents of both factors. The majority of trace element anomalies are related to the sites affected by the A-factor.  相似文献   

12.
用可见分光光度法与等离子体发射光谱法对仙人掌果汁色素及其微量元素的含量进行了测定,仙人掌果汁色素含量达2.1% ̄3.3%,成熟果的果汁色素含量比预成熟果大。在27种被测定的元素中,除As、Be、Cd、Co、Mo、Pb,Sb,Tl等未被检出外,其余Ag,Al,B,Ba,Ca,Cr,Cu,Fe,Mg,Mn,Na,Ni,Se,V,Zn,K,P,S等均有准确测定值。成熟果与预成熟果的果汁微量元素含量无明显  相似文献   

13.
Major, minor, trace and ultratrace concentrations of Ag, Al, As, Au, Ba, Be, Br, Ca, Cd, Ce, Cl, Co, Cr, Cs, Cu, Dy, Eu, Fe, Ga, Hf, K, La, Li, Lu, Mg, Mn, Na, Nb, Ni, P, Pb, Sb, Sc, Se, Sm, Sn, Sr, Ta, Th, Ti, U, V, W and Zn in crude juice, principal juice, sirup juice (produced during the successive stages of sugar industry), sugar cane plant, molasses, deposits (produced as a result of the addition of Ca(OH)2 and superphosphate and passage of SO2 through juice), A-and B-sugar and soil samples have been determined by destructive and nondestructive instrumental neutron activation (INAA), atomic absorption spectrophotometric (AAS) and inductively coupled plasma-atomic emission spectrometric (ICP-AES) analyses. The results obtained by the methods applied are in excellent agreement. Concentrations of the elements are different. Variations in element concentrations in cance plants and in crude juice may be attributed to composition changes or different botanical structures; in mixed juice, sirup, molasse and deposits they may be due to chemical treatments or corrosion effects on containers, whereas in soil samples to geochemical and biogeochemical fractionation as a result of adsorption and uptake of trace elements by plants from surrounding soil solutions.  相似文献   

14.
建立微波消解-电感耦合等离子体发射光谱(ICP-OES)测定汽车涂料中Pb,Cr,Se,Ba,Sb,As,Cd,Hg含量的方法。以HNO_3-H_2O_2(体积比为4∶1)混合酸消解样品,各元素分析谱线:Pb 220.353 nm,Cr 267.716 nm,Se196.090 nm,Ba 233.527 nm,Sb 217.581 nm,As 189.042 nm,Cd 228.802 nm,Hg 184.950 nm。8种元素测定结果的相对标准偏差为2.02%~12.94%(n=6);对白色、蓝色、红色汽车漆样品进行加标回收试验,Pb,Cr,Se,Ba,As,Cd,Hg,的加标回收率为81.26%~99.79%,Sb的回收率为62.43%~87.61%。该方法快速、简便,精密度、准确度较高,可用于汽车涂料中重金属含量的监控。  相似文献   

15.
采用微波灰化技术消化原油样品,并使用电感耦合等离子体原子发射光谱法(ICP-AES)测定其中Na、Mg、Ca、Fe、V、Ni和Cu的含量。探讨了原油样品中金属元素测定的称样量和微波灰化程序,并优化了仪器工作参数和实验条件。样品经微波灰化处理后,用盐酸溶解残渣,方法对Na、Mg、Ca、Fe、V、Ni和Cu元素的检出限分别为0.07、0.01、0.01、0.01、0.02、0.04和0.03mg/kg,回收率在84.5%~96.6%之间,相对标准偏差在2.1%~6.9%范围。方法简便、可靠,可用于原油中Na、Mg、Ca、Fe、V、Ni和Cu 7种金属元素的检测。  相似文献   

16.
ICP中钨基体对三十种元素的光谱干扰   总被引:2,自引:0,他引:2  
万家亮  金泽祥 《分析化学》1989,17(11):1031-1032,1030
  相似文献   

17.
A procedure is developed for determination of As, Co, Se, Cr, Pb, Zn, Cu, Mn, Cd, Sb, and Sn in water by ICP-AES analysis of alcohol eluates after pre-concentration of the samples. The pre-concentration is performed on a sodium diethyldithiocarbamate supported soft polyurethane foam. The sorbed elements are subsequently eluted with 1-propanol and the alcohol eluates are analysed by ICP-AES. A eight-fold concentration is achieved. An increased sensitivity in the analysis of propanol-water (30:70, v/v) solution is established as compared with aqueous solutions. The strongest effect is observed for As, Se, Pb, Cr, Sn, and Cd-increasing is more than twice. For other elements the matrix influence is by a factor of 1.45 (Cu), 1.36 (Sb), 2.08 (Zn). The method is applied to the analysis of natural water samples.  相似文献   

18.
Samples of the mosses Hylocomium splendens and Pleurozium schreberi, collected in the summer of 1998, were used to study the atmospheric deposition of heavy metals and other toxic elements in the Chelyabinsk Region situated in the South Urals, one of the most heavily polluted industrial areas of the Russian Federation. Samples of natural soils were collected simultaneously with moss at the same 30 sites in order to investigate surface accumulation of heavy metals and to examine the correlation of elements in moss and soil samples in order to separate contributions from atmospheric deposition and from soil minerals. A total of 38 elements (Na, Mg, Al, K, Ca, Sc, Ti, V, Cr, Mn, Fe, Co, Ni, Zn, As, Se, Rb, Sr, Zr, Mo, Sb, Cs, Ba, La, Ce, Nd, Sm, Eu, Gd, Tb, Dy, Yb, Hf, Ta, W, Au, Th, U) in soil and 33 elements Na, Mg, Al, Cl, K, Ca, Sc, V, Cr, Mn, Fe, Co, Ni, Zn, As, Se, Br, Rb, Ag, Sb, Cs, Ba, La, Ce, Sm, Tb, Yb, Hf, Ta, W, Au, Th, U) were determined by epithermal neutron activation analysis. The elements Cu, Cd and Pb (in moss samples only) were obtained by atomic absorption spectrometry. VARIMAX rotated principal component analysis was used to identify and characterize different pollution sources and to point out the most polluted areas.  相似文献   

19.
An instrumental neutron activation analysis method, using both reactor flux and epi-cadmium neutrons, has been developed for the determination of major, minor and trace elements in sub-seabed sediments. The method involves two different irradiations followed by three different counting periods using high-resolution Ge(Li) and low-energy photon detectors. The list of elements determined includes Ag, Al, As, Ba, Br, Ca, Ce, Cl, Co, Cr, Cs, Dy, Eu, Fe, Ga, Gd, Hf, Hg, I, In, K, La, Lu, Mg, Mn, Mo, Na, Nd, Ni, Pt, Rb, Re, Rh, Sb, Sc, Se, Si, Sm, Sn, Sr, Ta, Tb, Th, Ti, Tm, U, V. W, Yb, Zn, and Zr. The accuracy of the method has been evaluated by analyzing four different standard reference materials. The method has been applied to core samples collected from the Great Meteor East and the South Nares Abyssal Plain which are being evaluated as potential sites for the possible disposal of vitrified highly active waste.  相似文献   

20.
The concentration of As, Ba, Ca, Co, Cr, Cs, Dy, Eu, Fe, Ga, Hf, K, La, Lu, Mn, Mo, Na, Ni, Rb, Sb, Sc, Se, Sm, Sr, Ta, Tb, Th, U, Yb, and Zn were determined by instrumental neutron activation analysis in block shale samples of the New Albany Group (Devonian-Mississippian) in the in the Illinois Basin. Uranium content of the samples was as high as 75 ppm and interfered in the determination of samarium, molybdenum, barium and cerium. In the determination of selenium a correction was made for interference from tantalum. U, As, Co, Mo, Ni and Sb as well as Cu, V and pyritic sulphur which were determined by other methods, were found to correlate positively with the organic carbon content of the samples.  相似文献   

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