电感耦合等离子体原子发射光谱(ICP-AES)法测定锡铅焊料中11种微量元素

根据目前市场上常见锡铅焊料中主元素的特性(锡含量范围0.X%~95%,铅含量范围X%~99%),合理选择了有效的样品前处理方法。参考铸造锡铅焊料牌号及化学成分和仪器工作条件,确定了待测元素的测定范围。应用电感耦合等离子体原子发射光谱法同时测定锡铅焊料中锑、铋、铁、砷、铜、银、锌、铝、镉、磷、金11种元素的含量,方法操作简单。选择了合适的分析谱线,进行了基体元素对待测元素以及各待测元素之间的干扰研究,基体效应小,各待测元素之间基本无干扰,11次独立的测定数据相对标准偏差为1.0%~11.3%,方法的加标回收率为90.2%~105%。完全能满足现实生产中对锡铅焊料杂质元素的测定要求。     

Multielement analysis of housewares and other food-related items by a 241Am radioisotope X-ray fluorescence transportable spectrometer and handheld analyzers

Radioisotopic X-ray fluorescence spectrometry (RXRFS) performed with an analyzer based on a 241Am excitation source was investigated as a potential field method for screening housewares for the presence of toxic elements. A compact system based on commercially available detection and multichannel analyzer components was used to measure surface concentrations of Au, Ba, Bi, Cd, Ce, Co, Cs, Cu, Fe, La, Pb, Sb, Sn, Sr, Zn, and Zr in a wide variety of housewares and other food-related items. Certified reference material solders, glasses, and paint films and well-characterized oven-fired test tile glazes, solders, and metal can seams were analyzed to determine element sensitivities and analytical limits and to demonstrate the accuracy of the instrument. With analysis times of 3-5 min, the analyzer demonstrated 3sigma limits of detection of < or = 100 microg/cm2 for elements with Z = 40-65 and Z > 70. Very good accuracy was demonstrated for glaze and thin-sample analyses, whereas analysis was possible for solders and metal can seams with greater uncertainties (20-40%). Two commercially available handheld RXRFS analyzers, evaluated as part of the study, yielded results that agreed well with those obtained with the 124Am-based RXRFS system.     

黑苦荞保健茶中重金属的分析评价

采用原子吸收光谱法和原子荧光光度法测定了四川省凉山州某几个品牌黑苦荞保健茶中的重金属铅、镉、铬、无机砷和汞的含量,并以NY/T 1510-2007标准绿色食品麦类制品为依据,对黑苦荞保健茶重金属污染状况进行了分析评价。结果表明,黑苦荞保健茶受重金属元素污染的程度由高到低表现为铅、铬、镉、无机砷和汞,但含量均未超过国家标准规定;黑苦荞叶芽茶和全株茶的重金属污染较为严重,全胚茶未受重金属污染。     

Sesbania drummondii cell cultures: ICP-MS determination of the accumulation of Pb and Cu

Sesbania cell cultures grown in the presence of different concentrations of Pb (0-1000 mg/L) and Cu (0-500 mg/L) were assayed for growth, metal accumulations and activities of antioxidative enzymes: superoxide dismutase (SOD), catalase (CAT) and guaiacol peroxidase (GPX). These cultures tolerated Pb up to a concentration of 500 mg/L, registering a fresh weight growth of 500% in 3 weeks. At the same time, cultures registered a growth of 200% in 3 weeks at a Cu concentration of 100 mg/L showing less tolerance than Pb. However, Sesbania cells accumulated more Cu than Pb, as determined by ICP-MS, at all the treatments tested. Cu accumulation reached 3000 mg/kg (dry weight) at a Cu treatment of 100 mg/L, while Pb accumulation was only over 150 mg/kg (dry weight) at 500 mg Pb/L. Metal accumulations were positively correlated with induction of SOD and CAT activities in both the metal treatments. SOD activity of callus was 105 U/mg (fresh weight) at a Pb treatment of 500 mg/L and the corresponding Pb accumulation of 160 mg/kg (dry weight), while the activity rose to 300 U/mg (fresh weight) at a Cu treatment of 100 mg/L and the corresponding Cu accumulation of 3000 mg/kg (dry weight). The pattern of GPX activities was, however, different, particularly in Pb treatments where activities declined with increasing concentrations of Pb in the cells as well as growth medium. This study shows how Sesbania cells withstand heavy metal stress by induction of antioxidative enzyme activities.     

Determination of Toxic Elements in Soft Drinks by ICP-AES

The determination of toxic elements in food and beverages is very important as it has a major implication on toxicology and nutritional value. Addition of flavourings, preservatives and colourants during the manufacturing process can sometimes increase the level of toxic elements in processed food and beverages. Metal cans are most likely to also increase the level of some elements like Fe, Al, Zn and Pb through corrosion and rough handling during transporting and extended exposure to direct sunlight.     

Toxic and essential metals determination in commercial seafood: Paracentrotus lividus by ICP-MS

Toxic and essential metals content was determined by inductively coupled plasma mass spectrometry in commercial sea urchins samples from the Mediterranean Sea and Pacific Ocean. Results show that Chilean samples have the highest values of Cd, As, Ni, Cr and V; Spanish samples have the maximum Hg content while Sicilian samples have the lowest content of toxic metals. The toxic metal traces were compared with the limits of European Community (EC) No. 1881/2006 for bivalve molluscs. All samples exceed Pb and Cd limit levels; regarding Hg levels, only Sicilian and Sardinian samples have Hg content below the EC limits. The dietary intake of toxic and essential elements was evaluated for an adult. Furthermore, our study highlights a correlation between the toxic elements content and the marine environmental conditions of the places of origin even though only the generic FAO fishing area is specified.     

火焰原子吸收光谱法测定蝴蝶藤中六种金属元素的含量

中药蝴蝶藤对溃疡性结肠炎有显著疗效,为了解其治疗作用,用原子吸收光谱法测定了蝴蝶藤中6种金属元素的含量,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此样品中的金属元素Fe、Cu、Zn、Mn、Ca、Pb的含量进行了测定。结果表明,蝴蝶藤中Fe、Cu、Zn、Mn、Ca、Pb含量分别为26.732、9.762、17.164、21.576、1 923.412、0.234μg.mL-1,加样回收率为97.1%～102.7%。该法操作简单、结果准确,是蝴蝶藤中微量元素检测的理想方法。     

复合塑料包装袋中重金属迁移量的测定

将复合塑料袋用4％乙酸浸泡,采用石墨炉原子吸收光谱仪对其中的铅、镉、铬、镍、铜、砷迁移量进行了测定.结果表明:各元素的吸光度与质量浓度呈良好的线性关系,相关系数为0.998 9～0.9999,元素Pb、Cd、Cr、Ni、Cu、As的检出限分别为1.04、0.05、0.98、1.00、0.97、0.96 μg/L,各元素...     

Evaluation of Platanus occidentalis and Pinus sylvestris as bioindicators for lead and cadmium by slurry sampling-electrothermal atomic absorption spectrometry

Two higher plants (Platanus occidentalis and Pinus sylvestris) were used as bioindicators for assessment of contamination by Pb and Cd in an urban and industrialized area. Both toxic metals in plant tissue were determined by transverse-heated electrothermal atomic absorption spectrometry-longitudinal Zeeman background correction combined with automated ultrasonic slurry sampling. Twenty sampling points were established to observe a relationship between metal concentration in plant and traffic density. Screening optimization of variables influencing slurry preparations (sonication time, sonication power, and surfactant concentration) followed a fractional factorial design at 2 levels. No significant effects were observed in the interval of variables studied. Limits of detection of Pb and Cd in the plants were 0.28 and 0.025 microg/g (dry weight), respectively. Metal concentrations in the plants were in the range of 5-51 and 0.05-0.7 microg/g for Pb and Cd, respectively. Factor analysis to data of metal concentration in both plants, extractable metal content in soil, distance to traffic, and traffic density, showed a significant association between features such as concentration of Pb and Cd in leaves of P. occidentalis and traffic density, which accounted for the largest variance. Other features such as extractable metal contents in soil accounted for lesser variance, meaning that soils in the area investigated were less suitable than plants for monitoring metal pollution caused by vehicular traffic.     

Enhancing microdialysis recovery of metal ions by incorporating poly-l-aspartic acid and poly-l-histidine in the perfusion liquid

A study of the evaluation of poly-l-aspartic acid and poly-l-histidine as binding agents to enhance microdialysis recovery of metal ions is presented. Investigations were carried out to compare microdialysis recovery for Cr, Cu, Ni, and Pb when using water as the perfusion liquid as well as when using various concentrations of poly-l-aspartic acid and poly-l-histidine in the perfusion liquid. All experiments were carried out under quiescent conditions using a concentric type of microdialysis probe fitted with a polysulfone membrane having a 30 kDa molecular weight cut-off and a 10 mm effective dialysis length. The metal ions were determined using an electrothermal atomic absorption spectrometer equipped with a Zeemann background corrector. Incorporation of 0.032% (w/v) of poly-l-aspartic acid enhanced the recovery of Cu and Pb by factors of 90 and 64%, respectively (%RSD<3). The recovery of Cr was enhanced by 5%, but that of Ni never exceeded values achieved using ultra pure water. The use of 20% (w/v) of poly-l-histidine resulted in enhancement factors of 66 and 4% for Cu and Pb, respectively (%RSD<2). For both Cr and Ni, the recovery never exceeded that achieved with water. The data from these studies demonstrate the suitability of poly-l-aspartic and poly-l-histidine as selective and effective binding agents that enhance the microdialysis recovery of metal ions. Application of the optimised conditions to the determination of Pb and Cu in a wastewater sample confirmed the versatility of microdialysis, as higher recoveries of Cu were obtained with poly-l-aspartic acid compared to direct determination.     

石墨炉原子吸收光谱法测定含盐食品中铅

含盐食品样品经硝酸和过氧化氢加热消解,采用石墨炉原子吸收光谱法测定其中铅的含量。以氯化钯-硝酸铵为混合基体改进剂,灰化温度为1 200℃,原子化温度为1 850℃。铅(Ⅱ)的质量浓度在25μg·L-1以内与其吸光度呈线性关系,检出限(3s/b)为26pg。应用此法分析了酱油样品,加标平均回收率为96.2%,相对标准偏差(n=5)为3.0%。     

Modification of sodium aluminum silicate hydrate by thioglycolic acid as a new composite capable of removing and preconcentrating Pb(II), Cu(II), and Zn(II) ions from food and water samples

In this paper, sodium aluminum silicate hydrate was synthesized using rice husk as a silicon source and scrap aluminum cans as an aluminum source. Afterward, with the aid of microwave heating, a composite of sodium aluminum silicate hydrate and (3-aminopropyl)trimethoxysilane was facilely synthesized then modified by thioglycolic acid to produce a new composite. Besides, characterization of the synthesized composite was carried out using XRD, FT-IR, TEM, CHN elemental analyzer, nitrogen gas sorption analyzer, and SEM. The XRD pattern of the produced composite shows that there is a halo at 2θ = 25.0°, which means that there is a crystalline structure that is combined with an amorphous background. The SEM and TEM studies indicate that the synthesized composite has a structure similar to cotton. The synthesized composite was utilized for the efficient removal and preconcentration of Pb(II), Cu(II), and Zn(II) ions from food and water samples prior to determination by flame atomic absorption spectrometry. The produced composite has a maximum adsorption capacity of 185.53, 168.92, and 125.94 mg/g for Pb(II), Cu(II), and Zn(II) ions, respectively. The recovery findings demonstrate that the process is accurate, adaptable, and resulted in quantitative separation (greater than95 percent). Furthermore, the % RSD was less than 3.5 percent, indicating good reproducibility. The Langmuir isotherm and pseudo-second-order model fit the experimental results well. The thermodynamic studies established that the adsorption process is spontaneous, chemical, and exothermic. The produced composite was successfully regenerated and used multiple times to remove the metal ions under investigation from aqueous solutions.     

Phenolic compounds,antioxidant activity and Cu,Zn, Cd and Pb content in wild and cultivated cranberries and blueberries

The aim of this study was to determine the content of Cu, Zn, Cd and Pb and the total polyphenol (TP) content as well as the total antioxidant capacity (TAC) in wild cranberries and blueberries collected from different localities of the Slovakia and to compare them with properties of six cranberry and six highbush blueberry cultivars obtained from the research centre. Compared with cultivated cranberries (Cu, Zn, Cd and Pb content: 0.642, 1.496, 0.015 and 0.050 mg/kg FM) in wild fruits, higher Cu (by 37%) and lower Zn, Cd and Pb (by 8%, 7% and 44% respectively) were determined using atomic absorption spectrometry method. In wild blueberries, higher Cu, Zn and Pb (by 16%, 209% and 80% respectively) and similar Cd contents were determined compared with cultivated fruits (Cu, Zn, Cd and Pb content: 0.483, 0.541, 0.003 and 0.055 mg/kg FM). The TP contents estimated by spectrophotometry using Folin–Ciocalteau reagent were in intervals 1405–3161 (cranberries) and 1300–3077 (blueberries) expressed as mg GAE/kg FM. While the average TP content determined in wild cranberries was by 31% lower than that in cultivated cranberries, in wild blueberries it was by 97% higher compared with highbush blueberry cultivars. The values of TAC determined by spectrophotometry method using 2,2-diphenyl-1-picrylhydrazyl were in range 20.67–22.22 (cranberries) and 14.03–24.79 (blueberries) expressed as mmol TE/kg FM. In wild cranberries and blueberries, the lower average TAC values compared with cultivated berries were determined (by 1% and 28%, respectively).     

Mercury speciation and total trace element determination of low-biomass biological samples

Current approaches to mercury speciation and total trace element analysis require separate extraction/digestions of the sample. Ecologically important aquatic organisms--notably primary consumers such as zooplankton, polychaetes and amphipods--usually yield very low biomass for analysis, even with significant compositing of multiple organisms. Individual organisms in the lower aquatic food chains (mussels, snails, oysters, silversides, killifish) can also have very low sample mass, and analysis of whole single organisms is important to metal uptake studies. A method for the determination of both methyl Hg and total heavy metal concentrations (Zn, As, Se, Cd, Hg, Pb) in a single, low-mass sample of aquatic organisms was developed. Samples (2 to 50 mg) were spiked with enriched with (201)MeHg and (199)Hg, then leached in 4 M HNO(3) at 55 degrees C for extraction of MeHg. After 16 h, an aliquot (0.05 mL) was removed to determine mercury species (methyl and inorganic Hg) by isotope dilution gas chromatography inductively coupled plasma mass spectrometry (ICP-MS). The leachate was then acidified to 9 M HNO(3) and digested in a microwave at 150 degrees C for 10 min, and total metal concentrations were determined by collision cell ICP-MS. The method was validated by analyzing five biological certified reference materials. Average percent recoveries for Zn, As, Se, Cd, MeHg, Hg(total) and Pb were 99.9%, 103.5%, 100.4%, 103.3%, 101%, 97.7%, and 97.1%, respectively. The correlation between the sum of MeHg and inorganic Hg from the speciation analysis and total Hg by conventional digestion of the sample was determined for a large sample set of aquatic invertebrates (n = 285). Excellent agreement between the two measured values was achieved. This method is advantageous in situations where sample size is limited, and where correlations between Hg species and other metals are required in the same sample. The method also provides further validation of speciation data, by corroborating the sum of the Hg species concentrations with the total Hg concentration.     

Direct sample introduction of wines in graphite furnace atomic absorption spectrometry for the simultaneous determination of arsenic, cadmium, copper and lead content

A multi-element graphite furnace atomic absorption spectrometry (GFAAS) method was elaborated for the simultaneous determination of As, Cd, Cu, and Pb in wine samples of various sugar contents using the transversally heated graphite atomizer (THGA) with end-capped tubes and integrated graphite platforms (IGPs). For comparative GFAAS analyses, direct injection (i.e., dispensing the sample onto the IGP) and digestion-based (i.e., adding oxidizing agents, such as HNO(3) and/or H(2)O(2) to the sample solutions) methods were optimized with the application of chemical modifiers. The mixture of 5 microg Pd (applied as nitrate) plus 3 microg Mg(NO(3))(2) chemical modifier was proven to be optimal for the present set of analytes and matrix, it allowing the optimal 600 degrees C pyrolysis and 2200 degrees C atomization temperatures, respectively. The IGP of the THGA was pre-heated at 70 degrees C to prevent the sputtering and/or foaming of sample solutions with a high organic content, dispensed together with the modifier solution, which method also improved the reproducibility of the determinations. With the digestion-based method, the recovery ranged between 87 and 122%, while with the direct injection method it was between 96 and 102% for Cd, Cu, and Pb, whereas a lower, compromise recovery of 45-85% was realized for As. The detection limits (LODs) were found to be 5.0, 0.03, 1.2, and 0.8 microg l(-1) for As, Cd, Cu, and Pb, respectively. The characteristic mass (m(0)) data were 24 pg As, 1.3 pg Cd, 13 pg Cu, and 35 pg Pb. The upper limits of the linear calibration range were 100, 2, 100, and 200 microg l(-1) for As, Cd, Cu, and Pb, respectively. The precisions were not worse than 4.8, 3.1, 3.7, and 2.3% for As, Cd, Cu, and Pb, respectively. For arsenic, a higher amount of the modifier (e.g., 20 microg Pd plus 12 microg Mg(NO(3))(2)) could be recommended to overcome the interference from the presence of sulphate and phosphate in wines. Although this method increased the sensitivity for As (m(0)=20 pg), it also enhanced the background noise, thus only a slight improvement in the LOD of As (3.9 microg l(-1)) was realized. For the 35 red and white wine samples studied, the highest metal contents were observed for Cu ranging from 20 to 640 microg l(-1) (average: 148 microg l(-1)), followed by Pb from 6 to 90 microg l(-1) (average: 32.3 microg l(-1)), and Cd from 0.05 to 16.5 microg l(-1) (average: 1.06 microg l(-1)), whereas the As content was below the LOD. This wide fluctuation in the trace metal content could be associated with the origin of wines from various regions (i.e., different trace metal level and/or quality of soil, and/or anthropogenic impact), and with diverse materials (e.g., additives and containers) involved in the wine production processes. The Cu content of wine samples was significantly correlated with Pb, whereas its weak anti-correlation was found with Cd. Interestingly, the level of Pb was anti-correlated with the year of production of the wines. This is likely due to the gradual decrease in the Pb content of soils of vineyards by time, which certainly causes less Pb-uptake of the grape plant, thus a decrease in the Pb content of wines as well.     

Determination of metal content in valerian root phytopharmaceutical derivatives by atomic spectrometry

Phytopharmaceuticals containing Valerian are used as mild sleep-inducing agents. The elemental composition of 3 different marks of Valeriana officinalis roots commercially available in the Argentinian market, their teas, and a commercial tincture have been studied. The content of Al, Ca, Cd, Co, Cr, Cu, Fe, Li, Mn, Ni, Pb, V, and Zn was determined in phytopharmaceuticals by flame atomic emission/absorption spectrometry, electrothermal atomic absorption spectrometry, and ultrasonic nebulization coupled to inductively coupled plasma-optical emission spectrometry. Prior to analyses of the samples, a digestion procedure was optimized. The analytical results obtained for Fe, Al, Ca, and V in the solid sample study were within the range 100-1000 mg/kg, and for Mn, Zn, and Pb within the range 10-100 mg/kg. Cadmium was found at levels up to 0.0125 mg/kg.     

Extractive desulfurization of fuel oil with metal-based ionic liquids

Several metal-based ionic liquids (ILs) were synthesized and used as extractants for the desulfurization of dibenzothiophene (DBT) in simulated fuel oil. The effects of several anion and metal ions, n(ILs)/n(metal) as mole ratio, V_IL/V_oil and extractive times on the removal ratio of DBT were investigated in detail. The results showed that [BMIM]HSO₄/FeCl₃(BMIM was short for 1-butyl-3-methyl imidazole) was superior to the other ILs for the extractive desulfurization. A total of 100% of DBT was removed at room temperature in 5 min with V_[BMIM]HSO₄=FeCl₃=V_oil=1:1. The extractive activity of [BMIM]HSO₄/FeCl₃ IL did not change almost after five runs. Extractive desulfurization of different sulfur compounds and commercial diesel fuel oil were also examined. The removal ratios of the sulfur compounds as the reaction substrates were all over 90% and the sulfur content of commercial diesel oil decreased to 120 ppm from 12,400 ppm.     

Cellulose based macromolecular chelator having pyrocatechol as an anchored ligand: synthesis and applications as metal extractant prior to their determination by flame atomic absorption spectrometry

Pyrocatechol is immobilized on cellulose via ---NH---CH₂---CH₂---NH---SO₂---C₆H₄---N=N--- linker and the resulting macromolecular chelator characterized by IR, TGA, CPMAS ¹³C NMR and elemental analyses. It has been used for enrichment of Cu(II), Zn(II), Fe(III), Ni(II), Co(II), Cd(II) and Pb(II) prior to their determination by flame atomic absorption spectrometry (FAAS). The pH ranges for quantitative sorption (98.0–99.4%) are 4.0–7.0, 5.0–6.0, 3.0–4.0, 5.0–7.0, 5.0–8.0, 7.0–8.0 and 4.0–5.0, respectively. The desorption was found quantitative with 0.5 mol dm⁻³ HCl/HNO₃ (for Pb). The sorption capacity of the matrix for the seven metal ions has been found in the range 85.3–186.2 μmol g⁻¹. The optimum flow rate of metal ion solution for quantitative sorption of metal onto pyrocatechol functionalized cellulose as determined by column method, is 2–6 cm³ min⁻¹, whereas for desorption it is 2–4 cm³ min⁻¹. The tolerance limits for NaCl, NaBr, NaI, NaNO₃, Na₂SO₄, Na₃PO_4, humic acid, EDTA, ascorbic acid, citric acid, sodium tartrate, Ca(II) and Mg(II) in the sorption of all the seven metal ions are reported. Ascorbic acid is tolerable up to 0.8 mmol dm⁻³ with Cu and Pb where as sodium tartrate does not interfere up to 0.6 mmol dm⁻³ with Pb. There is no interference of NaBr, NaCl and NaNO₃ up to a concentration of 0.5 mol dm⁻³, in the sorption of Cu(II), Cd(II) and Fe(III) on to the chelating cellulose matrix The preconcentration factors are between 75 and 300 and t_1/2 values ≤5 min for all the metal ions. Simultaneous sorption of Cu, Zn, Ni and Co is possible at pH 5.0 if their total concentration does not exceed lowest sorption capacity. The present matrix coupled with FAAS has been used to enrich and determine the seven metal ions in river and tap water samples (relative standard deviation (R.S.D.) 1.05–7.20%) and synthetic certified water sample SLRS-4 (NRC, Canada) with R.S.D. 2.03%. The cobalt present in pharmaceutical vitamin tablets was also preconcentrated on the modified cellulose and determined by FAAS (R.S.D. 1.87%).     

常见茶叶中14种元素含量分析及重金属风险评价

采集传统名茶地标产品样品各3种为实验样品,通过ICP-OES和ICP-MS对样品进行K、Ca、Mg、Mn、B、Cu、Fe、Ni、Zn、Cr、Co、Cd、As、Pb等14种元素的含量测定.利用单因素方差分析、主成分分析、污染评价等方法,对茶叶无机元素含量进行分析和污染评价,并对污染来源进行了研究.结果表明,不同产地茶叶样...     

广州市孕妇头发微量元素含量测定

测定了286例不同孕周孕妇头发锌、铁、铜、钙、锰、铅含量,并进行了比较分析。结果表明,孕期上述元素的异常率分别为：40．21％、37．76％、15．04％、45．46％、19．58％、27．97％。不同孕周变化各有差异,以孕中期变化最为明显（除铜和锰外,P＜0．01）。提示妊娠期妇女有益微量元素缺乏的现象是很普遍的,妊娠中晚期事理调整膳食结构和营养物质的补充是必要的。