Determination of lead in soil samples by in-valve solid-phase extraction–flow injection flame atomic absorption spectrometry

Sooksamiti, Ponlayuth; Geckeis, Horst; Grudpan, Kate

doi:10.1039/an9962101413

Cited by 36 publications

(16 citation statements)

References 19 publications

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“…As it has been reported [17,19,21,22] that the sorption characteristics of the resin for lead are affected by the concentration of nitric acid, the concentration of nitric acid in the carrier solution was varied over a range. This range was 0-20% (v/v) for manifold 1, and 0-5% (v/v) for manifold 2.…”

Section: Methods Developmentmentioning

confidence: 99%

Evaluation of Pb-Spec® for flow-injection solid-phase extraction preconcentration for the determination of trace lead in water and wine by flame atomic absorption spectrometry

Bakırcıoğlu

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et al. 2003

Analytica Chimica Acta

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Two manifold designs were evaluated. Water samples and wine digests in 10% nitric acid were pumped through a column containing a commercially available resin (Pb-Spec ® ), an immobilized crown ether with a cavity size selective for Pb 2+ . The column was rinsed with 2% HNO 3 and the eluent, 0.1 mol l −1 ammonium oxalate was injected via a six-port rotary valve. The eluted lead was delivered to the flame atomic absorption spectrometer at 4.0 ml min −1 . The following flow-injection (FI) parameters were optimized: sample acidity and volume, loading and elution flow rates, and eluent composition and volume.The detection limit for the water samples, estimated from the noise on the signal obtained for 250 ml of 10 g l −1 loaded at 19.1 ml min −1 was 1 g l −1 . For 50 ml of wine digest loaded at 4 ml min −1 , the value was 3 g l −1 . The roles of loading flow rate and sample volume were investigated in detail. The variation in retention efficiency with loading flow rate showed that the amount of lead retained (during a fixed loading time) increased with flow rate until the upper performance limit of the peristaltic pump was reached. The variation of detection limit with sample volume followed the expected hyperbolic relationship and showed that only small improvements in LOD were obtained for volumes greater than 50 ml. The method was evaluated through spike recovery for both water and wine. The lead contents of tap (0.24 g l −1 ), pond (0.40 g l −1 ), and river waters (not detected) were determined. The concentrations of lead in three Port wine samples ranged from not detected to 190 g l −1 . No significant matrix suppression effects were observed.

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Section: Methods Developmentmentioning

confidence: 99%

Evaluation of Pb-Spec® for flow-injection solid-phase extraction preconcentration for the determination of trace lead in water and wine by flame atomic absorption spectrometry

Bakırcıoğlu

Segade

Yourd

et al. 2003

Analytica Chimica Acta

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“…The detection limit equivalent to 3σ of the background signal was 0.05 µg of lead, so that the detection limit in concentration is 0.5 ppb Pb when 100 ml of a sample solution is injected. Sooksamiti et al 11 have reported that the detection limit (3σ) was 0.08 µg of lead and an RSD of 4.1 % was achieved for 0.8 µg of lead(II) (n=15). The superiority of our data over those by Sooksamiti et al can probably be ascribed to our use of a noise filter to reduce the signal noise.…”

Section: The Effect Of the Sample Volume Injected And Repeatabilitymentioning

confidence: 99%

On-line Preconcentration and Determination of Lead in Iron and Steel by Flow Injection-Flame Atomic Absorption Spectrometry

et al. 2000

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High purity iron has recently received much attention as a new material with excellent characteristics. 1,2 The development of reliable analytical methods for the determination of trace impurity elements are required for production of pure iron. On the other hand, the use of scrap iron is increasing to make use of resources effectively and the accurate determination of various impurity metals in iron and steel is therefore essential for the quality control of iron products.The detection limit of lead by flame atomic absorption spectrometry (FAAS) is about 10 ng/ml. 3 Therefore the determination of traces of lead in high purity metals by FAAS usually requires its preconcentration, in addition to the separation of lead from matrix elements. Generally the blank value introduced from the reagents or from the laboratory environment must be kept at as low a level as possible in order to obtain the precise analytical results for traces of lead.Flow injection (FI) on-line preconcentration procedures now play an important role in trace metal analysis. They offer the possibility of determining lower analyte concentrations and avoiding matrix effects by separation of the analyte from interfering matrix components. Furthermore the consumption of time, sample and reagent, and the risk of contamination from the laboratory environment are low; the repeatability and efficiency are high compared with its corresponding batch counterpart procedures. [4][5][6][7] In this respect, FI systems combined with ion exchange or solid phase extraction techniques carried out in minicolumns have been successfully used in flame atomic absorption spectrometry (FAAS) because the preconcentrated analytes can be simply eluted into the nebulizer. [5][6][7][8] A large variety of highly efficient sorbents are usually used in on-line techniques for determination of trace metals, as reviewed by Yebra-Biurrum. 9 These sorbents include inorganic activated alumina; ion exchangers modified with complexing reagents; sorbents based on silica gel, naphthalene, styrenedivinylbenzene copolymers (XAD), and porous glass beads with immobilized chelates groups; reversed-phase silica sorbent (C18, C16 and C8); activated carbon; and chelating resins and celluloses. The typical chelating resin, Chelex-100, with iminodiacetate chelating groups has been among the most used. These sorbents are mostly used for determination of trace metal ions in natural water, biological samples, and food, but in some cases, these samples bring about difficulties if they contain large amounts of metal ions. For example, this problem gets complicated when trace elements are determined in complex metallic matrix samples such as waste water, alloys and rocks, because the column adsorbs not only micro components but also some matrix elements like iron, copper and others as well, and the sorbent capacity is insufficient.This work was undertaken to examine a Pb-selective chromatographic resin, 10 Pb·Spec TM (EIChrom Industries), to preconcentrate and separate lead from other sample matrix comp...

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“…[23][24][25][26] The commercially available immobilized crown ether (Pb-Spec and Sr-Spec resin) has been used for preconcentration of lead in various matrices. 27,28 The physical immobilization of crown ether on the knotted reactor has been also used for preconcentration and separation of palladium in tunnel dust. 29 However, to the best of our knowledge, reports on physical immobilization of crown ethers on solid supports used as the sorbent for preparation of column or microcolumn of solid phase extraction of metal ions is rare.…”

Section: Introductionmentioning

confidence: 99%

Determination of thallium traces by ETAAS after on-line matrix separation and preconcentration in a flow injection system

Asadoulahi¹,

Dadfarnia²,

Shabani³

2007

J. Braz. Chem. Soc.

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Um sistema de injeção em fluxo sensível e simples foi desenvolvido para separação, pré-concentração e determinação de tálio. A pré-concentração é baseada na sorção do analito em uma microcoluna de dibenzo-18-coroa-6 (DB18C6) imobilizada em alumina revestida com surfactante e subseqüente eluição com solução de ácido nítrico (500 µL, 2 mol L -1 ). A concentração de tálio no eluente foi determinada por espectrometria de absorção atômica com atomização eletrotérmica. Os fatores que influenciaram a sorção e dessorção de íon tálio foram investigados. Para um volume da amostra de 5 mL, a calibração foi linear no intervalo de 0,1 a 20 µg L -1 (r = 0,9996) com um limite de detecção de 0,05 µg L -1 . A capacidade máxima de sorção foi de 1432 µg de tálio por grama do sorbente. A precisão do método para 1 µg L -1 foi 5,7% RSD (n = 11). O método foi aplicado para determinação de tálio em água, cabelo, unha e em materiais de referência certificados. A exatidão foi avaliada empregando experimentos de adição e recuperação ou por comparação dos resultados com materiais de referência certificados.A simple and sensitive flow injection system was developed for separation, preconcentration and determination of thallium. Preconcentration is based on the analyte sorption on a microcolumn of dibenzo-18-crown-6 (DB18C6) immobilized on surfactant coated alumina with subsequent elution using a nitric acid solution (500 µL, 2 mol L -1 ). The concentration of thallium in the eluent was determined using electrothermal atomic absorption spectrometry. Factors influencing the sorption and desorption of thallium ion were investigated. Using a sample volume of 5 mL, the calibration was linear from 0.1 to 20 µg L -1 range (r = 0.9996) with a detection limit of 0.05 µg L -1 . The maximum sorption capacity was 1432 µg of thallium per gram of sorbent. The precision of the method at 1 µg L -1 was 5.7% RSD (n = 11). The method was applied for determination of thallium in water, hair, nail, and standard reference samples. The accuracy was assessed using addition-recovery experiment or by comparison of the results with certified reference materials.

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Determination of lead in soil samples by in-valve solid-phase extraction–flow injection flame atomic absorption spectrometry

Cited by 36 publications

References 19 publications

Evaluation of Pb-Spec® for flow-injection solid-phase extraction preconcentration for the determination of trace lead in water and wine by flame atomic absorption spectrometry

Evaluation of Pb-Spec® for flow-injection solid-phase extraction preconcentration for the determination of trace lead in water and wine by flame atomic absorption spectrometry

On-line Preconcentration and Determination of Lead in Iron and Steel by Flow Injection-Flame Atomic Absorption Spectrometry

Determination of thallium traces by ETAAS after on-line matrix separation and preconcentration in a flow injection system

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