Simultaneous pre-concentration procedure for the determination of cadmium and lead in drinking water employing sequential multi-element flame atomic absorption spectrometry

In this paper is proposed a simultaneous pre-concentration procedure using cloud point extraction for the determination of cadmium and lead in drinking water employing sequential multi-element flame atomic absorption spectrometry. The ligand used is 2-(2-thiazolylazo)-p-cresol (TAC) and the micellar phase is obtained using non-ionic surfactant octylphenoxypolyethoxyethanol (Triton X-114) and centrifugation.The optimization step was performed using two-level factorial design and Doehlert design. A multiple response function was established in order to get experimental conditions for simultaneous extraction of cadmium and lead.The method allows the determination of cadmium and lead with detection limits of 0.077 μg L^− 1 and 1.05 μg L^− 1 respectively, precision expressed as relative standard deviation (RSD) of 1.5 and 3.3% (n = 10) for cadmium concentrations of 30 μg L^− 1 and 50 μg L^− 1, respectively, and RSD of 1.8% and 2.7% for lead concentrations of 30 μg L^− 1 and 50 μg L^− 1, respectively. The accuracy was confirmed by analysis of a certified reference material of natural water.This method was applied for the determination of cadmium and lead in drinking water samples collected in Jaguaquara City, Brazil. Tests of addition/recovery were also performed for some samples and results varied from 95 to 104% for cadmium and 96 to 107% for lead. The cadmium and lead concentrations found in these samples were always lower than the permissible maximum levels stipulated by Brazilian Health Organization.     

Cloud point extraction for the determination of cadmium and lead employing sequential multi-element flame atomic absorption spectrometry

A cloud point extraction procedure for pre-concentration and determination of cadmium and lead in drinking water using sequential multi-element flame atomic absorption spectrometry is described. 4-(2-thiazolylazo)-orcinol (TAO) has been used as complexing agent and the micellar phase was obtained using the non-ionic surfactant octylphenoxypolyethoxyethanol (Triton X-114) and centrifugation. The conditions for reaction and extraction (surfactant concentration, reagent concentration, effect of incubation time, etc) were studied and the analytical characteristics of the method were determined. The method allows the determination of cadmium and lead with quantification limits of 0.30?µg?L^?1 and 2.6?µg?L^?1, respectively. A precision expressed as relative standard deviation (RSD, n?=?10) of 2.3% and 2.6% has been obtained for cadmium concentrations of 10?µg?L^?1 and 30?µg?L^?1, respectively, and RSD of 1.3% and 1.7% for lead concentrations of 10?µg?L^?1 and 30?µg?L^?1, respectively. The accuracy was confirmed by analysis of a natural water certified reference material. The method has been applied for the determination of cadmium and lead in drinking water samples collected in the cities of Ilhéus and Itabuna, Brazil. Recovery tests have also been performed for some samples, and results varied from 96 to 105% for cadmium and 97 to 106% for lead. The cadmium and lead concentrations found in these samples were always lower than the permissible maximum levels stipulated by World Health Organization and the Brazilian Government.     

Rapid coprecipitation-separation and flame atomic absorption spectrometric determination of lead and cadmium in water with cobalt (II) and ammonium pyrrolidine dithiocarbamate

A coprecipitation technique which does not require complete collection of the precipitate was proposed for the determination of trace lead and cadmium in water with flame atomic absorption spectrometry (FAAS) after preconcentration of lead and cadmium by using cobalt (II) and ammonium pyrrolidine dithiocarbamate (Co-APDC) as coprecipitant and known amount of cobalt as an internal standard. Since lead, cadmium and cobalt were well distributed in the homogeneous precipitate, the concentration ratio of lead to cobalt, and cadmium to cobalt remained unchanged in any part of the precipitate. The amount of lead and cadmium in the original sample solution can be calculated respectively from the ratio of the absorbance values of lead and cadmium to cobalt in the final sample solution that is measured by FAAS and the known amount of the lead and cadmium in the standard series solutions. The optimum pH range for quantitative coprecipitation of lead and cadmium is from 3.0 to 4.5. The 16 diverse ions tested gave no significant interferences in the lead and cadmium determination. Under optimised conditions, lead ranging from 0 to 40?µg and cadmium ranging from 0 to 8?µg were quantitatively coprecipitated with Co-APDC from 100?mL sample solution (pH?～?3.5). This coprecipitation technique coupled with FAAS was applied to the determination of lead and cadmium in water samples with satisfactory results (recoveries in the range of 94.0–108%, relative standard deviations <6.0%).     

Coprecipitation of lead and cadmium using copper(II) mercaptobenzothiazole prior to flame atomic absorption spectrometric determination

A coprecipitation method using a combination of 2-mercaptobenzothiazole (MBT) as a chelating reagent and copper as the coprecipitate carrier is described for the determination of trace lead and cadmium by flame atomic absorption spectrometry. The coprecipitation conditions, such as the effect of pH, the amount of carrier element and reagent, standing time, sample volume and matrix effects were examined in detail. It was found that lead and cadmium are coprecipitated quantitatively (≥95%) with Cu(II)-MBT at pH 9 and that the relative standard deviations (n = 7) were ≤1.6%. When using the enrichment factors of 150-fold for lead and cadmium, the detection limits (3s/b) obtained are 1.08 for lead and 0.04 μg L⁻¹ for cadmium. The method was validated with spiked sea water, stream water, well water, and vegetable samples.     

Determination of zinc and copper in human hair by slurry sampling employing sequential multi-element flame atomic absorption spectrometry

The present work proposes a direct method based on slurry sampling for the determination of zinc and copper in human hair samples by multi-element sequential flame atomic absorption spectrometry. The slurries were prepared by cryogenic grinding and sonication of the samples. The optimization step was performed using univariate methodology and the factors studied were: nature and concentration of the acid solution, amount sample/slurry volume, sonication time, and particle size. The established experimental conditions are the use of a sample mass of 50 mg, 2 mol L^− 1 nitric acid solution, sonication time of 20 min and slurry volume of 10 mL. Adopting the optimized conditions, this method allows the determination of zinc and copper with detection limits of 88.3 and 53.3 ng g^− 1, respectively, and precision expressed as relative standard deviation (RSD) of 1.7% and 1.6% (both, n = 10) for contents of zinc and copper of 100.0 and 33.3 μg g^− 1, respectively. The accuracy was checked and confirmed by analysis of two certified reference materials of human hair. The procedure was applied for the determination of zinc and copper in two human hair samples. The zinc and copper contents varied from 100.0 to 175.6 and from 3.2 to 32.8 μg g^− 1, respectively. These samples were also analyzed after complete digestion in a closed system and determination by FAAS. The statistical comparison by t-test (95% confidence level) showed no significant difference between these results.     

火焰原子吸收光谱法间接测定药剂中的核黄素

本文利用高碘酸钠对相邻羟基氧化作用的专属性,在一定介质中,高碘酸钠与核黄素完全反应后,过量的高碘酸的钠与硝酸铅或者硝酸铜生成沉淀,通过测定Pb<'2+>或者Cu<'2+>,建立了间接测定核黄素含量的方法.铅体系和铜体系测定的相对标准偏差(RSD)分别为4.8%和5.2%,检出限分别为0.6μg.mL<'-1>和0.5μ...     

饮用水中痕量银的聚合物改性硅胶固相萃取-火焰原子吸收光谱法测定

研究了以聚异丁烯-alt-马来酸酐和L-半胱氨酸改性硅胶固相萃取-原子吸收光谱法(SPE-FAAS)测定饮用水中痕量银的方法;考察了样品pH、进样体积、流速,以及洗脱剂种类、浓度、体积、流速等参数对萃取率的影响,同时研究了共存离子的影响,评价了萃取材料的吸附容量及再生性能.结果表明,在优化的实验条件下,该法的检出限(3σ)为1.5μg.L-1,相对标准偏差(RSD)为2.9%(c=20μg.L-1,n=7),富集倍数为18.7.该法可成功地用于测定井水、自来水、纯净水等水样中的痕量银.     

On-line determination of manganese in solid seafood samples by flame atomic absorption spectrometry

Manganese is extracted on-line from solid seafood samples by a simple continuous ultrasound-assisted extraction system (CUES). This system is connected to an on-line manifold, which permits the flow-injection flame atomic absorption spectrometric determination of manganese. Optimisation of the continuous leaching procedure is performed by an experimental design. The proposed method allows the determination of manganese with a relative standard deviation of 0.9% for a sample containing 23.4 μg g⁻¹ manganese (dry mass). The detection limit is 0.4 μg g⁻¹ (dry mass) for 30 mg of sample and the sample throughput is ca. 60 samples per hour. Accurate results are obtained by measuring TORT-1 certified reference material. The procedure is finally applied to mussel, tuna, sardine and clams samples.     

双硫腙螯合型树脂同时分离富集-火焰原子吸收光谱法测定痕量铅和镉

以大孔聚苯乙烯树脂为母体,通过-N=N-,与双硫腙键合,合成了双硫腙螯合型树脂,并将其应用于痕量铅和镉的同时分离富集,实验了酸度、流速、共存离子干扰等因素对双硫腙螯合型树脂吸附和洗脱Pb和Cd的影响,建立了双硫腙螯合型树脂同时分离富集-火焰原子吸收光度法测定食品及环境样品中痕量Pb和Cd的方法.对Pb和Cd,方法的检出限分别为0.015和0.0013μg/mL,相对标准偏差(RSD)均优于3.0%.     

Cloud point extraction of aluminum (III) in water samples and determination by electrothermal atomic absorption spectrometry,flame atomic absorption spectrometry and UV-visible spectrophotometry

Cloud point extraction was applied as a preconcentration step for the determination of trace level of Al(III) in water samples with electrothermal atomic absorption spectrometry (ETAAS), flame atomic absorption spectrometry (FAAS) and UV-visible spectrophotometry. The aluminum was extracted as aluminum-Eriochrome Cyanine R (ECR) complex, at pH 6 by micelles of the non-ionic surfactant octylphenoxypolyethoxyethanol (Triton X-114). The investigations showed that the same CPE procedure can be used for different detection techniques. The results obtained from these techniques were evaluated. Under the optimal conditions, limit of detection obtained with ETAAS, FAAS and UV-visible spectrophotometry were 0.03 ng mL^?1, 0.06 µg mL^?1 and 0.01 µg mL^?1, respectively. The accuracy of the procedure was tested by analysing certified reference material. The method was successfully applied to determination of aluminum in water samples and dialysis fluid.     

Determination of cadmium in tobacco smoke and zinc in tap water by solvent extraction flame atomic absorption spectrometry

Procedures are described for the determination of cadmium in tobacco smoke and zinc in tap water by flame atomic absorption spectrometry after chelation with benzyl 2-pyridyl ketone 2-pyridylhydrazone and extraction with isobutyl methyl ketone. Calibration graphs in the organic layer were linear up to 1.3 g/ml, with sensitivities of 80 ng/ml (Zn) and 71ng/ml (Cd), and limits of detection of 49 ng/ml for zinc and 38 ng/ml for cadmium. RSD values were 2.9% at 0.42 g/ml (Cd) and 4.7% at 0.17 g/ml (Zn).     

On-line solid phase extraction coupled to flame atomic absorption spectrometry for the determination of trace copper and zinc in environmental and biological samples

In this work, bamboo charcoal (BC) was used as a sorbent for on-line solid phase extraction (SPE) coupling with flame atomic absorption spectrometry (AAS) for trace copper and zinc determination in environmental and biological samples. Under the optimum pH of 5.5 (for Zn) and 7.0 (for Cu), trace copper and zinc were effectively adsorbed on the microcolumn and the retained cations were efficiently eluted with HCl or HNO₃ with an appropriate concentration and flow rate for on-line AAS determination. With a sample loading time of 60 s at a sample flow rate of 7.6 mL min^?1, the enhancement factors of 39 (for Cu) and 30 (for Zn) and detection limits (3σ) of 0.60 µg L^?1 (for Cu) and 0.36 µg L^?1 (for Zn), respectively, were achieved. The sample throughput was 45 h^?1. At the level of 20 µg L^?1of Cu(II) and Zn(II), the precision (RSD, n?=?11) were found to be 0.26% and 1.6%, respectively. The proposed method has been successfully applied to the determination of copper and zinc in environmental and biological samples.     

Improvements in thermospray flame furnace atomic absorption spectrometry

In thermospray flame furnace atomic absorption spectrometry (TS-FF-AAS) a nickel atomization tube is placed in the acetylene/air flame on a holder built onto a standard AAS burner head. The liquid to be analyzed is transported by a low or high-pressure pump through a very hot, simple, inexpensive ceramic capillary tip acting as a flame-heated thermospray into the flame furnace. This results in complete sample introduction and increases the residence time of the sample in the absorption volume. This leads for 17 elements to a 3-110-fold improvement in the power of detection compared to conventional flame AAS. The absolute detection limits (3s values, N=25) lie between 0.2 μg l⁻¹ (Zn) and 310 μg l⁻¹ (Se) according to the element. The R.S.D. (N=15) is 1.4-5.5% according to the element and applied concentration. TS-FF-AAS can easily be incorporated on any standard flame AAS instrument and can be automated with a standard autosampler.     

Temperature-controlled ionic liquid-liquid-phase microextraction for the pre-concentration of lead from environmental samples prior to flame atomic absorption spectrometry

Hydrophobic ionic liquid could be dispersed into infinite droplets under driving of high temperature, and then they can aggregate as big droplets at low temperature. Based on this phenomenon a new liquid-phase microextraction for the pre-concentration of lead was developed. In this experiment, lead was transferred into its complex using dithizone as chelating agent, and then entered into the infinite ionic liquid drops at high temperature. After cooled with ice-water bath and centrifuged, lead complex was enriched in the ionic liquid droplets. Important parameters affected the extraction efficiency had been investigated including the pH of working solution, amount of chelating agent, volume of ionic liquid, extraction time, centrifugation time, and temperature, etc. The results showed that the usually coexisting ions containing in water samples had no obvious negative effect on the recovery of lead. The experimental results indicated that the proposed method had a good linearity (R = 0.9951) from 10 ng mL⁻¹ to 200 ng mL⁻¹. The precision was 4.4% (RSD, n = 6) and the detection limit was 9.5 ng mL⁻¹. This novel method was validated by determination of lead in four real environmental samples for the applicability and the results showed that the proposed method was excellent for the future use and the recoveries were in the range of 94.8-104.1%.     

Cloud point extraction procedure for flame atomic absorption spectrometric determination of lead(II) in sediment and water samples

The conditions for cloud point extraction of lead(II) from aqueous solutions were investigated and optimized. The procedure is based on the separation of Pb(II) – brillant cresyl blue (BCB) complexes into the micellar media by adding the surfactant Triton X-114. After phase separation, the surfactant-rich phase was dissolved with 1 mol L⁻¹ HNO₃ in ethanol and diluted with 1 mol L⁻¹ HNO₃ solution before lead was determined by flame atomic absorption spectrometry. Optimization of the pH, ligand and surfactant quantities, incubation time, temperature, viscosity, sample volume, and interfering ions was performed. The effects of the matrix ions were also examined. The detection limits for three times the standard deviations of the blank for lead were 7.5 μg L⁻¹ for water samples and 0.33 μg g⁻¹ for sediment samples. The validity of cloud point extraction was checked by employing certified reference samples of Lake Sediment IAEA-SL-1 and Sewage Sludge BCR-CRM 144R. The procedure was applied to natural waters and sediment samples with satisfactory results (recoveries >95%, relative standard deviations <6.4%).     

Fast sequential multi-element determination of major and minor elements in environmental samples and drinking waters by high-resolution continuum source flame atomic absorption spectrometry

The fast sequential multi-element determination of 11 elements present at different concentration levels in environmental samples and drinking waters has been investigated using high-resolution continuum source flame atomic absorption spectrometry. The main lines for Cu (324.754 nm), Zn (213.857 nm), Cd (228.802 nm), Ni (232.003 nm) and Pb (217.001 nm), main and secondary absorption lines for Mn (279.482 and 279.827 nm), Fe (248.327, 248.514 and 302.064 nm) and Ca (422.673 and 239.856 nm), secondary lines with different sensitivities for Na (589.592 and 330.237 nm) and K (769.897 and 404.414 nm) and a secondary line for Mg (202.582 nm) have been chosen to perform the analysis. A flow injection system has been used for sample introduction so sample consumption has been reduced up to less than 1 mL per element, measured in triplicate. Furthermore, the use of multiplets for Fe and the side pixel registration approach for Mg have been studied in order to reduce sensitivity and extend the linear working range. The figures of merit have been calculated and the proposed method was applied to determine these elements in a pine needles reference material (SRM 1575a), drinking and natural waters and soil extracts. Recoveries of analytes added at different concentration levels to water samples and extracts of soils were within 88–115% interval. In this way, the fast sequential multi-element determination of major and minor elements can be carried out, in triplicate, with successful results without requiring additional dilutions of samples or several different strategies for sample preparation using about 8–9 mL of sample.     

微波消解-火焰原子吸收法测定猪肝脏中的铅

采用微波消解—火焰原子吸收法对猪肝脏(鲜)中的痕量铅进行了测定,建立了一种微波消解样品、火焰原子吸收法测定猪肝脏(鲜)中痕量铅含量的方法.研究结果表明,在取样量为0.8g左右、HNO3(65％)∶H2O2(30％)=1∶1(体积比)、中等微波功率消解3 min的条件下,检测到猪肝脏中铅的含量为0.173 μ g/g.该...     

Indirect flow-injection determination of ascorbic acid by flame atomic absorption spectrometry

A continuous-flow procedure is proposed for the indirect determination of ascorbic acid, based on its reducing properties because of the oxidation of its 1,2-enediol group. Iron(III) was injected into a 1,10-phenanthroline stream, which was mixed with a sample carrier and then with a sodium picrate solution stream. In these conditions the iron(III) was reduced to iron(II) by the ascorbic acid. Thus, the iron(II) formed reacts with 1,10-phenanthroline to form a charged red complex, which with picrate ion forms a stable red-orange uncharged ion-association complex that is adsorbed on-line on a non-ionic polymeric adsorbent (Amberlite XAD-4), proportionally to the ascorbic acid in the sample. The unadsorbed iron was determined by flame atomic absorption spectrometry. The proposed method allows the determination of ascorbic acid in the range 0.5–25 g ml^–1 with a relative standard deviation of 2.9% at a rate of ca. 90 samples h^–1. This method has been applied to the determination of ascorbic acid in pharmaceutical preparations, fruit juices and sweets. The results obtained in the analysis are compared with those provided by the 2,6-dichloroindophenol method.     

Comparison of action of mixed permanent chemical modifiers for cadmium and lead determination in sediments and soils by slurry sampling graphite furnace atomic absorption spectrometry

Slurry sampling atomic absorption spectrometry with electrothermal atomization was used to the determination of cadmium (Cd) and lead (Pb) in soils and sediments using permanent modifiers. Comparison of action of mixed permanent modifiers niobium (Nb)/iridium (Ir) and tungsten (W)/iridium (Ir) were studied in detail. The effect of amount of Ir, W and Nb on analytical signals of Cd and Pb was examined. The optimal amounts of modifiers for Cd and Pb determination were stated. Niobium carbide formation on graphite surface was studied for different pyrolysis temperatures. Finally for Cd determination in sediments and soils 200 μg of Nb mixed with 5 μg of Ir was used as permanent modifiers and 15 μg of Nb mixed with 200 μg of Ir for Pb determination. Suspensions were prepared in 5% HNO₃. The analytical procedure was optimized carefully basing on data from pyrolysis and atomization curves studies. Ammonium dihydrogen phosphate was used additionally as matrix modifier during Cd determination in samples in order to prevent interferences coming from matrix components. The analysis of CRMs confirmed the reliability of the proposed approach. The precision and accuracy of Cd and Pb determination by the described method for soils and sediments were acceptable.     

Uncertainty of atomic absorption spectrometry: Application to the determination of lead in blood

The major sources of uncertainty of a method for determination of Pb in whole blood by atomic absorption spectrometry were identified. The combined uncertainty was compared to the experimentally determined variation and a satisfactory agreement was found, indicating that no significant sources of uncertainty have been overlooked and that the method is in a state of statistical control. The findings suggest that the major source of uncertainty at low concentrations are random fluctuations (noise) of the atomic signal. Therefore, if improvement of the method performance is needed, only actions directed towards enhancing the signal-to-noise ratio are suitable.