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.     

石墨炉原子吸收光谱法间接测定蒸汽含水率

利用石墨炉子吸收光谱法测定蒸汽发生器循环水和蒸汽冷凝水中的铯则间接测定蒸汽含水率。蒸汽含水率等于冷凝水中铯的浓度除以循环水中铯的浓度。石墨炉原子吸收光谱可以准确测定０．１ｇ／Ｌ至１ｍｇ／Ｌ浓度的铯,样品中可能存在的一些物质对测定没有干扰。本方法可以满足测定蒸汽含水率的要求,实现了数百份含水率样品的测试。     

Determination of cobalt in biological samples by line-source and high-resolution continuum source graphite furnace atomic absorption spectrometry using solid sampling or alkaline treatment

Two procedures for the determination of Co in biological samples by graphite furnace atomic absorption spectrometry (GF AAS) were compared: solid sampling (SS) and alkaline treatment with tetramethylammonium hydroxide (TMAH) using two different instruments for the investigation: a conventional line-source (LS) atomic absorption spectrometer and a prototype high-resolution continuum source atomic absorption spectrometer. For the direct introduction of the solid samples, certified reference materials (CRM) were ground to a particle size ≤50 μm. Alkaline treatment was carried out by placing about 250 mg of the sample in polypropylene flasks, adding 2 mL of 25% m/v tetramethylammonium hydroxide and de-ionized water. Due to its unique capacity of providing a 3-D spectral plot, a high-resolution continuum source (HR-CS) graphite furnace atomic absorption spectrometry was used as a tool to evaluate potential spectral interferences, including background absorption for both sample introduction procedures, revealing that a continuous background preceded the atomic signal for pyrolysis temperatures lower than 700 °C. Molecular absorption bands with pronounced rotational fine structure appeared for atomization temperatures >1800 °C probably as a consequence of the formation of PO. After optimization had been carried out using high resolution continuum source atomic absorption spectrometry, the optimized conditions were adopted also for line-source atomic absorption spectrometry. Six biological certified reference materials were analyzed, with calibration against aqueous standards, resulting in agreement with the certified values (according to the t-test for a 95% confidence level) and in detection limits as low as 5 ng g⁻¹.     

Determination of manganese, iron and copper in sodium by chemical modification/graphite furnace atomic absorption spectrometry

Trace Mn, Fe and Cu in sodium were determined by chemical modification/graphite furnace atomic absorption spectrometry. The sodium sample was changed into NaOH in a desiccator by room temperature water vapor generated under reduced pressure, then the NaOH was dissolved in water and HNO(3) was added to give a clear solution. The solution was analysed by chemical modification/graphite furnace atomic absorption spectrometry. A nickel nitrate modifier was effective in improving integrated absorbance signals and the reproducibility of measurement. Analytical results for Mn, Fe and Cu were 170, 970 and 210 ng/g and relative standard deviations (n = 5) were 3.5, 5.8 and 6.7%, respectively. These results agreed with the values obtained from a chelating resin preconcentration/ICP-AES method.     

嵌段分子筛聚合材料P123-SH萃取分离-石墨炉原子吸收光谱法分析痕量铬的形态

研究了嵌段分子筛聚合材料P123-SH萃取分离-石墨炉原子吸收光谱法对尿中痕量铬的形态分析方法,探讨了嵌段分子筛聚合材料P123-SH吸附铬的原理和最佳条件。在pH 7.0、常温下,Cr3+和Cr(Ⅵ)被很好的分离,且Cr3+可被该材料定量吸附,其吸附容量为6.15 mg/g。吸附的Cr3+可用2 mol/L的HCl洗脱,用石墨炉原子吸收法测定洗脱下来的Cr3+,往溶液中加入0.1%抗坏血酸将Cr(Ⅵ)还原为Cr3+测总铬,Cr(Ⅵ)含量为总铬减去Cr3+,方法测定Cr3+的检出限为0.011μg/L(3σ,n=11),线性范围为0.1～10μg/L,加标回收率在94%～106%之间,对0.50μg/L的Cr3+溶液平行测定7次,RSD为3.6%。方法可应用于生物样品和环境样品中痕量铬的形态分析。     

Selective determination of ultra trace amounts of gold by graphite furnace atomic absorption spectrometry after dispersive liquid-liquid microextraction

A simple, rapid and sensitive method is proposed for selective determination of ultra trace amounts of gold from different samples. The method is based on highly efficient separation and pre-concentration of gold by dispersive liquid-liquid microextraction of gold followed by its determination with graphite furnace atomic absorption spectrometry. The pre-concentration procedure results in quantitative extraction of gold by victoria blue R from a 10-mL sample into fine droplets of chlorobenzene, with a sedimented volume of 25 microL. Then, 20 microL of 0.04% Pd(NO3)2, as chemical modifier, followed by 10 microL of the sedimented phase were consecutively pipetted into the same auto-sampler device and the content is injected into the graphite tube and the gold content is determined by graphite furnace atomic absorption spectrometry. After optimizing the extraction conditions and instrumental parameters, a pre-concentration factor of about 388 is obtained for the system. The analytical curve is linear in a concentration range of 0.03-0.5 ng mL(-1). The detection limit and relative standard deviation are 0.005 ng mL(-1) and 4.2%, respectively. The method was successfully applied to the extraction and determination of gold in tap water and silicate ore samples.     

二苯硫脲-醋酸丁酯萃取-石墨炉原子吸收法测定地球化学样品中痕量银

对石墨炉原子吸收光谱法测定地球化学样品中痕量银进行了研究。样品经盐酸、硝酸、硫酸、高氯酸溶解,在盐酸(1.2mol/L)介质中用醋酸丁酯萃取银与二苯硫脲螯合物,用石墨炉原子吸收光谱法测定地球化学样品中痕量银,方法检出限为0.011ng/mL,相对标准偏差(RSD,n=11)为6.0%~12.2%,加标回收率为96.00%~105.00%。能满足地球化学样品中银含量为0.02~5μg/g范围内银测定的准确度和精密度的要求。     

Study of Analytical Methods for Iron Determination in Complex Organic Liquids by Atomic Absorption Spectrometry

Abstract

In the determination of iron in complex organic liquids by atomic absorption spectrometry (A. A. S.), methods of sample preparation, such as dilution with an organic solvent and sample pretreatment to destroy organic material, are investigated. Moreover, methods of analysis using calibration curve and standard additions are presented. The possible cause of error associated with iron determination in organic samples by flame (F-A. A. S.) and graphite furnace (GF-A. A. S.) atomic absorption spectrometry are discussed.

From all of these studies, the use of graphite furnace atomic absorption spectrometry after sample dilution with methyl isobutyl ketone, and the use of the method of standard additions are advised for iron determination.     

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.     

Radioisotope X-ray fluorescence analysis of vanadium in petroleum coke samples

Radioisotope X-ray fluorescence spectrometry, RIXRF, was used for the determination of vanadium in Venezuelan petroleum coke samples using a simple standardless method and fundamental parameter approach. The values obtained by this method were in agreement with values measured by graphite furnace atomic absorption spectrometry, GFAAS.     

Coprecipitation Behavior of Some Metals with Chitosan and Their Determination by Graphite Furnace Atomic Absorption Spectrometry

Chitosan is derived from chitin by deacetylation. Chitosan forms a complex with metal ions and is soluble an organic acid. The metal ions were concentrated in the precipitates of chitosan when the sample solution containing metal ions was adjusted to neutral after the chitosan solution was added. These properties are applied to the preconcentration of metal ions in water samples and their determination by graphite furnace atomic absorption spectrometry. Metal ions,such as ruthenium, indium, vanadium, strontium,rhodium were collected in the chitosan precipitates.     

Differentiation of Spanish brandies according to their metal content

Eleven metals, namely, aluminium, calcium, cadmium, copper, iron, lead, magnesium, manganese, potassium, sodium and zinc were determined in twenty samples of Sherry brandies and twelve samples of Penedés brandies by applying atomic spectrometry techniques. Flame atomic absorption spectrometry was used for quantitating calcium, copper, iron, magnesium, manganese and zinc; atomic emission spectrometry to determine potassium and sodium; and graphite furnace atomic absorption spectrometry to analyse aluminium, cadmium and lead. A chemometric approach was followed to study the discrimination between brandies from Sherry or Penedés according to the metal profile.     

Solid phase extraction and graphite furnace atomic absorption spectrometric determination of ultra trace amounts of bismuth in water samples

A simple and reliable method for the selective extraction and determination of bismuth in water as well as alloy samples using octadecyl bonded silica cartridge modified with cyanex 301 and graphite furnace atomic absorption spectrometry is described. Extraction efficiency and influence of sample matrix, optimum amount of extraction ligand, type and least amount of proper eluent and flow rates were evaluated. The limit of detection of the proposed method is 0.01 ng ml(-1). The influence of potential interfering cations in water samples on the recovery of bismuth was investigated. The method was successfully applied to the extraction and determination of bismuth in natural water and alloy samples.     

Microwave oven samle dissolution for the analysis of environmental and biological materials

An HCl/HNO₃/HF PTFE bomb dissolution technique using microwave heating was tested on several environmental and biological materials. Nearly 25 elements in the dissolved samples were determined mainly by inductively coupled plasma—atomic emission spectrometry or graphite furnace atomic absorption spectrometry. Results of the analysis of several hundred samples are discussed.     

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…     

Trace and major element compositions of Black Sea aerosol

Instrumental neutron activation analysis (INAA), flame atomic absorption spectrometry (FAAS), flame atomic emission spectrometry (FAES), graphite furnace atomic absorption spectrometry (GF-AAS), ion chromatography (IC) and visible spectrometry (VIS) were used to determine the composition of atmospheric aerosols, collected at a rural site in the Western Black Sea Coast of Turkey. A total of 354 daily aerosol samples were analyzed for 46 trace and major elements and ions. Sample preparation, quality control procedures, instrumental operating conditions for INAA and source apportionment work is presented.     

Size exclusion chromatography of aluminium species in natural waters

Size exclusion chromatography was used in order to characterize organically bound aluminium in natural water samples. A Superose column was used, with 0.1 M acetate buffer (pH 4.6) as mobile phase. Three detection systems were used; graphite furnace atomic absorption spectrometry, post-column reaction with pyrocatechol violet and UV spectrometry at 254 nm. A single peak was obtained for organic aluminium in natural waters. The results indicated that aluminium binds with a broad size range of humic substances, and that the inorganic aluminium was present in polymeric form.     

Determination of antimony dopant and some ultra-trace elements in semiconductor silicon by atomic absorption spectrometry with introduction of solid samples into the furnace

Antimony as a dopant at a level of ca. 35 atom/10⁶ atoms (ppm, atomic) and ultra-trace concentrations of lead and manganese (<0.02 ppm, atomic) are determined in semiconductor silicon by atomic absorption spectrometry after introduction of milligram samples of silicon to a pyrolytically-coated graphite furnace. Calibration was done with standard aqueous solutions. Iron, silver, zinc and cadmium were sought but were at concentrations below the limits of detection. The graphite microboats used for sample introduction were useful for only 3–10 samples because of silicon carbide formation.     

Determination of indium by graphite furnace atomic absorption spectrometry after coprecipitation with chitosan.

A sensitive and simple method for the determination of trace amounts of indium in water samples by graphite furnace atomic absorption spectrometry (GFAAS) after coprecipitation with chitosan was investigated. Indium was quantitatively preconcentrated from water samples by coprecipitation with chitosan at pH 7.0-9.0. The coprecipitant was easily dissolved with acetic acid, and indium in the resulting solution was determined by GFAAS. The addition of lanthanum as a chemical modifier was more effective for the atomic absorbance of indium. The detection limit (S/N > or = 3) for indium was 0.04 microg dm(-3), and the relative standard deviations (n = 5) were 3.5-4.5% at 1.0 microg/100 cm3. The results obtained in this study indicate that the proposed method can be successfully applied to the determination of trace indium in water samples.     

原子吸收光谱法在烟草行业中的应用进展

对1961～2011年间3种类型的原子吸收光谱法,包括火焰原子吸收光谱法、石墨炉原子吸收光谱法和蒸气发生原子吸收光谱法在烟草行业中的应用进行了综述(引用文献63篇)。