藏药材铁棒锤的微量元素含量分析

目的研究藏药材铁棒锤的微量元素含量。方法使用电感耦合等离子体质谱仪(ICPMS)测定藏药材铁棒锤药材中As、Hg、Pb、Cd含量,使用原子吸收光谱仪(火焰法、石墨炉法)测定药材中Zn、Mn、Cr、Fe、Ca、K、Cu元素的含量并进行分析。结果铁棒锤中有害元素As、Hg、Pb、Cd含量较低,Cu、Fe等有益元素含量较高。结论藏药材铁棒锤有丰富的微量元素,具有较高的开发利用价值。     

芦蒿中六种金属微量元素含量的测定

为给芦蒿中微量元素的检测提供科学方法。采用浓硝酸微波消解法处理样品,用火焰原子吸收分光光度法和石墨炉法对芦蒿样品中的金属元素Fe、Cu、Zn、Mn、Ca、Pb的含量进行了测定。结果表明,方法的加样回收率为96.80%～103.04%。该法操作简单、结果准确,是芦蒿中微量元素检测的理想方法。     

枸杞、红枣中金属元素含量的测定

选用了中国宁夏中宁早康枸杞园林场生产的枸杞、山东省沾化金丝枣、山西柳林县红枣,用火焰原子吸收分光光度法[1]和石墨炉法对这三种样品中的金属元素Fe、Cu、Zn、Mn、Ca、Pb的含量进行了测定。测定方法简单,精密度和灵敏度高,回收率为105.1%~93.1%,结果可靠。     

Flow Injection Semi-online Preconcentration Graphite Furnace Atomic Absorption Spectrometry for Determination of Cadmium, Copper and Manganese

IntroductionGraphite furnace atomic absorption spectrome-try (GFAAS) is one of the most sensitive tech-niques for the determination of various elementswith detection limits in the range ofμg/ L to ng/ L.Despite the impressive detection power of the tech-nique,GFAAS can tbe routinely used to make di-rect analysis of some real samples with complexcomposition[1] . This is due to the matrix interfer-ence and/ or insufficient detection power. Conse-quently,separation and preconcentration proc…     

Determination of trace elements in lithium niobate crystals by solid sampling and solution-based spectrometry methods

Solid sampling (SS) graphite furnace atomic absorption spectrometry (GFAAS) and solution-based (SB) methods of GFAAS, flame atomic absorption spectrometry (FAAS), inductively coupled plasma optical emission spectrometry (ICP-OES) and inductively coupled plasma mass spectrometry (ICP-MS) were elaborated and/or optimized for the determination of Cr, Fe and Mn trace elements used as dopants in lithium niobate optical crystals.     

火焰和石墨炉原子吸收光谱法对大米中金属元素含量的测定分析

采用火焰和石墨炉原子吸收光谱法对随机抽取的江西省、吉林省共五种大米中的Fe、Cu、Zn、Mn、Ca、Pb等六种金属元素进行了测定。结果表明,江西省大米中的金属元素含量均略高于吉林省前谷县达里巴乡大米,这可能与南北土壤中金属元素的分布不同有关。     

Preconcentration of trace elements in potable liquids by means of a liquid membrane emulsion for flame atomic absorption determination

Summary A liquid membrane emulsion was developed for the simultaneous extraction and preconcentration of traces of Cd, Co, Cu, Fe, Mn, Ni, Pb and Zn in potable liquids. After preconcentration, the eight elements were determined by flame atomic absorption spectrometry (FAAS). The results of analyses of potable water, beer and soft drinks, each from five or six different sources are listed. Data from the preconcentration method were compared with corresponding data obtained from the direct determination of the elements by graphite furnace atomic absorption spectrometry (GFAAS). Differences in results for trace elements between the liquid membrane emulsion-FAAS method and the GFAAS method were in the ranges of ±10% (water), ±9% (beer) and ±14% (soft drinks) for most of the trace elements. The satisfactory agreement meant that analyses of such liquids for trace elements can be carried out accurately with less expensive and widely available FAAS equipment.     

Direct determination of traces of copper,zinc, lead,cobalt, iron and cadmium in bovine liver by graphite furnace atomic absorption spectrometry using the solid sampling and the platform techniques

A simple and rapid method is described for direct determination of traces of Cu, Zn, Pb, Co, Fe and Cd in NBS bovine liver, SRM 1577, by graphite furnace atomic absorption spectrometry. The solid sampling technique was used, thereby avoiding the dilution factor involved in the solution technique, and also the risk of contamination from the environment in sample handling and from reagents, solvents and vessels. The organic matrix was burnt off and removed by using a well-defined selective volatilization technique combined with the analyte modification technique. Also, the effect of the platform technique in removing matrix interferences was studied using an anisotropic pyrolytic graphite platform inside the commercial graphite tube. The results of the “with platform” and the “without platform” techniques were equally accurate, but the “with platform” technique gave better precision.     

Determination of lead, copper and manganese by graphite furnace atomic absorption spectrometry after separation/concentration using a water-soluble polymer

In this study, a water-soluble polymer, polyvinylpyrrolidinone (PVP) having chelating functionalities was used for the preconcentration and separation of traces of Pb, Cu, Ve and Mn prior to their determination by graphite furnace atomic absorption spectrometry. For this purpose, the sample and the PVP solutions were mixed and the metal bound polymer was precipitated by adding the mixture onto acetone. The precipitate was separated by decantation and dissolved with water. By increasing the ratio of the volumes of sample to water used in dissolving the precipitate, the analyte elements were concentrated as needed. The concentration of trace elements was determined using graphite furnace atomic absorption spectrometry. The analyte elements in matrix free aqueous solutions were quantitatively recovered. The validity of the proposed method was checked with a standard reference material (NIST SRM 1577b bovine liver) and spiked fruit juice, sea water and mineral water samples. The analytical results were found to be in good agreement with certified and added values. Detection limits (3δ) were 1.7, 3.6 and 4.1 μg l⁻¹ for Pb, Cu and Mn, respectively, using 10 μl of sample volume. The method is novel and can be characterized by rapidity, simplicity, quantitative recovery and high reproducibility.     

Human albumin as a reference material for trace elements

Summary An investigation through interlaboratory comparison using different analytical techniques has been carried out in order to assess the suitability of a plasma protein solution as a source for a trace element reference material in clinical analysis. Reasonable agreement was obtained for a number of elements from the range studied: Al, Ba, Cr, Cu, Fe, Mg, Mn, Mo, Ni, Se, Sr, V and Zn. The techniques used included flame and furnace atomic absorption spectrometry (FAAS and ETA-AAS), furnace atomic emission spectrometry (ETA-AES), inductively coupled plasma atomic emission spectrometry (ICP-AES), inductively coupled plasma mass spectrometry (ICP-MS), and simultaneous multi-element atomic absorption spectrometry (SIMAAC). Results indicated that this plasma protein solution may prove useful as a source for a reference material covering trace element levels outwith the range found in normal human plasma.

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Humanalbumin als Referenzmaterial für Spurenelemente

     

Determination of trace elements in Antarctic krill samples by inductively coupled atomic emission and graphite furnace atomic absorption spectrometry

Analytical methods were developed for the determination of trace elements in Antarctic krill samples applying inductively coupled plasma atomic emission spectrometry (ICP-AES) and graphite furnace atomic absorption spectrometry (GF-AAS). Cu, Fe, Mn and Zn were determined by ICP-AES, while Cd and Pb by GF-AAS technique. Two microwave assisted digestion procedures were elaborated for the preparation of 0.5-g krill samples using open and closed vessel systems. The efficiency of the digestion processes was checked by measurements of the total organic carbon content of the solutions obtained. The deviations of the analytical data from the certified values and the relative standard deviations of the concentration measurements were lower for all six elements investigated applying the closed vessel digestion system.     

三种蜂花粉中微量元素含量的测定分析

采用火焰和石墨炉原子吸收光谱法对荞麦蜂花粉、茶花蜂花粉和莲花蜂花粉中的六种金属元素Fe、Cu、Zn、Mn、Ca、Pb的含量进行了测定。方法简单,精密度和灵敏度高,回收率为98.30%~93.51%,结果可靠。     

Summary of preparation and homogeneity characterization of ten agricultural food reference materials for elemental composition

Summary Preparation and development has been completed of ten agricultural/food reference materials (RMs): bovine muscle powder, corn starch, hard red spring wheat flour, soft winter wheat flour, whole milk powder, wheat gluten, corn bran, durum wheat flour, whole egg powder and microcrystalline cellulose. Homogeneity tests for 14 elements, Al, Ca, Cd, Co, Cu, Fe, K, Mg, Mn, Na, Ni, Pb, Sr and Zn were performed by the initiating laboratories by application of precise and reliable analytical methods based on flame atomic absorption spectrometry and graphite furnace atomic absorption spectrometry. An extensive set of analytical results obtained from the interlaboratory cooperative characterization campaign was assessed to provide homogeneity estimates for other elements. Estimates of homogeneity from within-laboratory precision indicated that all materials exhibited acceptable homogeneity for virtually all 29 elements (Al, As, B, Ba, Br, Ca, Cd, Cl, Co, Cr, Cu, Fe, Hg, I, K, Mg, Mn, Mo, N, Na, Ni, P, Pb, Rb, S, Se, Sr, V, Zn) for which best estimate concentration values are available. Two thirds of all homogeneity coefficients of variation were below 5%.     

Determination of trace impurities in aluminum nitride by direct solid sampling graphite furnace atomic absorption spectrometry

The trace impurities Cr, Cu, Fe, K, Mn, Sb and Zn were determined in powdered aluminum nitride by direct solid sampling graphite furnace atomic absorption spectrometry using a ZEEnit 60 atomic absorption spectrometer. This spectrometer features inverse Zeeman-effect background correction and a variable magnetic field enabling measurements in two sensitivity modes over a concentration range of three orders of magnitude. The measurement sensitivity can be adjusted to the analyte concentration in the sample. The use of chemical modifiers was not necessary. Calibration was carried out by means of calibration curves obtained with aqueous standard solutions. Accuracy was checked mainly by comparison of the results with those obtained by instrumental and radiochemical neutron activation analysis whereby, excluding the results for potassium, no significant differences were found by carrying out the t-test at the significance level 0.05. The limits of detection were between 0.05 ng g⁻¹ (Zn) and 80 ng g⁻¹ (Fe) and the relative standard deviations below 11 %. With the proposed method, up to ten measurement cycles can be carried out in one hour.     

Multielement analysis of green coffee and its possible use for the determination of origin

Using instrumental neutron activation analysis (INAA), graphite furnace atomic absorption spectrometry (GFAAS), flame atomic absorption spectrometry (FAAS) and combustion elemental analysis, green coffees of the Arabica species produced in crop year 1987/88 in Colombia, Costa Rica, Cuba, El Salvador, Mexico, Nicaragua, Panamá and Papua New Guinea were analysed for the elements Ba, Br, C, Ca, Co, Cr, Cu, Cs, Fe, H, K, La, Mg, Mn, N, Na, Rb, Sc, Sr and Zn. In accordance with the concentrations determined, the elements could be ranked into five groups: Sc (sub-ppb level); Br, Co, Cr, Cs and La (ppb level); Ba, Cu, Fe, Mn, Na, Rb, Sr and Zn (ppm level); Ca and Mg (%o level); and C, H, K and N (% level). On the basis of the results obtained, an attempt was made to establish the origin of the green coffee via its elemental composition. Among the investigated elements, manganese was found to be best suited as an indicator for this purpose. However, the elements C, Co, Cs, Na and Rb proved to be of interest too.     

海水中铜锌铅镉的萃取-反萃取法同时提取-原子吸收光谱法测定

采用萃取-反萃取法同时提取出海水中Cu、Zn、Pb、Cd,Cu、Pb、Cd石墨炉法测定,Zn用火焰法测定.对样品的前处理方法和最佳仪器条件进行了研究,并通过加标实验验证了方法的可靠性.结果表明:萃取-反萃取法能完全满足海水中Cu、Zn、Pb、Cd的前处理要求,可节省一半前处理时间,有溶液稳定、环保、节省试剂等优点.     

Utilization of optimized BCR three-step sequential and dilute HCl single extraction procedures for soil-plant metal transfer predictions in contaminated lands

The prediction of soil metal phytoavailability using the chemical extractions is a conventional approach routinely used in soil testing. The adequacy of such soil tests for this purpose is commonly assessed through a comparison of extraction results with metal contents in relevant plants. In this work, the fractions of selected risk metals (Al, As, Cd, Cu, Fe, Mn, Ni, Pb, Zn) that can be taken up by various plants were obtained by optimized BCR (Community Bureau of Reference) three-step sequential extraction procedure (SEP) and by single 0.5 mol L(-1) HCl extraction. These procedures were validated using five soil and sediment reference materials (SRM 2710, SRM 2711, CRM 483, CRM 701, SRM RTH 912) and applied to significantly different acidified soils for the fractionation of studied metals. The new indicative values of Al, Cd, Cu, Fe, Mn, P, Pb and Zn fractional concentrations for these reference materials were obtained by the dilute HCl single extraction. The influence of various soil genesis, content of essential elements (Ca, Mg, K, P) and different anthropogenic sources of acidification on extraction yields of individual risk metal fractions was investigated. The concentrations of studied elements were determined by atomic spectrometry methods (flame, graphite furnace and hydride generation atomic absorption spectrometry and inductively coupled plasma optical emission spectrometry). It can be concluded that the data of extraction yields from first BCR SEP acid extractable step and soil-plant transfer coefficients can be applied to the prediction of qualitative mobility of selected risk metals in different soil systems.     

Cloud point extraction and graphite furnace atomic absorption spectrometry determination of manganese(II) and iron(III) in water samples

Cloud point extraction (CPE) was applied as a preconcentration step prior to graphite furnace atomic absorption spectrometry (GFAAS) determination of manganese(II) and iron(III) in water samples. After complexation with 1-phenyl-3-methyl-4-benzoyl-5-pyrazolone (PMBP), the analytes could be quantitatively extracted to the phase rich in the surfactant p-octylpolyethyleneglycolphenylether (Triton X-100) and be concentrated, then determined by GFAAS. The parameters affecting the extraction efficiency, such as solution pH, concentration of PMBP and Triton X-100, equilibration temperature and time, were investigated in detail. Under the optimum conditions, preconcentration of 10 ml of sample solution permitted the detection of 0.02 ng ml(-1) of Mn(II) and 0.08 ng ml(-1) of Fe(III) with enrichment factors of 31 and 25 for Mn(II) and Fe(III), respectively. The proposed method was applied to determination of trace manganese(II) and iron(III) in water samples with satisfactory results.     

Chemical vapor generation—electrothermal atomic absorption spectrometry: new perspectives

Volatile species of Ag, Cu, Cd, and Zn were generated at room temperature by the addition of sodium tetrahydroborate (III) to an acidified solution of the analytes. The vapor-phase species were rapidly transported to a pre-heated graphite tube, the surface of which was previously treated with Ir as a permanent chemical modifier. The volatile species were trapped at the Ir treated tube surface, and the further heating of the furnace permits their determination by atomic absorption spectrometry. A univariate approach was used to achieve optimized conditions and derive the figures of merit. The limits of detection based on a 3σ_b criterion were 10 (1); 0.006 (6×10⁻⁴); 28 (2.8) and 1.1 (0.11) ng (μg ml⁻¹) for Ag, Cd, Cu and Zn, respectively. Precision of replicate measurements was typically approximately 10% R.S.D. Using a transfer line as short as possible should minimize losses of analyte during the transport to the graphite furnace. The overall efficiency of the volatile species generation and trapping process estimated for silver was 13%.