Fast method of multi-elemental analysis of stream sediment samples by inductively coupled plasma-mass spectrometry (ICP-MS) with prior single-step microwave-assisted digestion

Roje, Vibor

doi:10.1590/s0103-50532011000300017

Cited by 10 publications

(14 citation statements)

References 11 publications

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“…Digestion II showed less variation in temperature. Roje 22 observed that even when there is little variation in the applied digestion temperature; it affects the extraction efficiency of the elements.…”

Section: Resultsmentioning

confidence: 99%

“…In operating temperature conditions of up to 230 °C, adopting a gradient of 1200 s, and maintained and cooled in two equal time periods, they achieved recovery rates of 99 % for Pb, with the 3051 method and of between 90 to 97 % with regia water (nitro hydrochloric acid) and of 105 % and 87 % using full digestion. 22,23 With operating temperatures of up to 200 °C, digestion in 1500 s, added cooling time of 900 s, 97 % and 98 % recovery rates were achieved with regia water. 24 Working with temperatures of up to 300 °C with complete and total digestion time of from 2160 s to 2940 s digestion, we obtained 90-102 % recovery.…”

Section: Resultsmentioning

confidence: 99%

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Evaluation of Analytical Methods for Lead (Pb) (USEPA 3051) and Zinc (Zn) (HR-CS AAS) in Sediments

et al. 2018

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Rev. Virtual Quim., 2018, 10 (3), 518-528. Data de publicação na Web: 28 de junho de 2018 http://rvq.sbq.org.br Avaliação de Métodos Analíticos de Pb (USEPA 3051) e de Zn (HR-CS AAS) em SedimentoResumo: Diversas técnicas de análise podem ser utilizadas para determinar a concentração de metais no sedimento, como os métodos 3050, 3051 e 3052 da United States Environmental Protection Agency (USEPA). A leitura de amostras após a digestão pode ser realizada em espectrometria de absorção atômica de alta resolução de fonte contínua (HR-CS AAS), e pode ser aplicada a técnica de correção de fundo pelo algoritmo de mínimos quadrados (LSBC). O presente estudo teve por objetivo testar os tempos de digestão (5000 s, digestão um e 1800 s, digestão dois) pelo método 3051, na determinação de Pb e corrigir possíveis interferências espectrais na determinação de Zn em amostras de sedimento pela LSBC. A amostragem foi realizada no Rio Palmeiras, afluente do Rio Tubarão, SC, Brasil. As amostras foram digeridas em forno de micro-ondas e leituras em HR-CS AAS, com atomização em chama. Para Pb, realizaram-se as leituras das amostras digeridas das digestões um e dois, e para Zn, realizaram-se as leituras apenas da digestão dois, sem e com a LSBC. Observaram-se menores variações de temperatura e maiores taxas de recuperação de Pb na digestão dois. O uso da LSBC nas leituras do Zn possibilitou a obtenção de valores mais acurados. Palavras-chave:Metais, Micro-ondas, Absorção atômica. AbstractA variety of analytical techniques may be used to determine the concentration of metals in sediment, such as methods numbers 3050, 3051 and 3052 of the United States Environmental Protection Agency (USEPA). The reading of samples after digestion can be carried out by high-resolution continuous source atomic absorption spectrometry (HR-CS AAS), and background correction technique can be applied by the squared minimums algorithm (LSBC). This study aims to test the digestion times (5000 s, for first digestion and 1800 s for second digestion) using the 3051 method, to determine the Pb level and correct possible spectral interferences in the determination of Zn in sediment samples by LSBC. Sampling was conducted in the Palmeiras River, a tributary of the River Tubarão, SC, Brazil. Samples were digested in microwave ovens and readings in HR-CS AAS with flaming atomization. Pb readings were found for the samples digested in number one and two digestions, and a Zn reading was found in only the second digestion, with and without LSBC. Minor variations in temperature were observed and higher Pb recovery rates were found in the second digestion. The use of LSBC in Zn readings made it possible to obtain more accurate values.

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Section: Resultsmentioning

confidence: 99%

Section: Resultsmentioning

confidence: 99%

Evaluation of Analytical Methods for Lead (Pb) (USEPA 3051) and Zinc (Zn) (HR-CS AAS) in Sediments

et al. 2018

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“…After the sludge sample was calcinated in the muffle furnace for 12 h at 700°C, 150 milligrams of sample were introduced into a vessel and 1 mL of the standard of 1000 mg L -1 of NiCl 2 was added in order to calculate the nickel recovery. The digestion was performed with 15 mL of a mixture of nitric acid and hydrochloric acid (3:1) using the microwave system which has reported recoveries higher than 90 % [23,24]. The vessel was then placed in the microwave oven set at a power of 900 W with an initial temperature of 50°C.…”

Section: Analytical Proceduresmentioning

confidence: 99%

Determination of artificial beta-emitters in sludge samples

Fonollosa

Nieto

Peñalver

et al. 2016

J Radioanal Nucl Chem

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A method has been developed for the determination of two artificial beta emitters ( 55 Fe and 63 Ni) in sludge samples from a drinking water treatment plant (DWTP). The activities found for 55 Fe and 63 Ni ranged between (\15 Bq kg -1 ) and 162 Bq kg -1 , and between (\10 Bq kg -1 ) and 65 Bq kg -1 , respectively. Using the sludge activities is possible to estimate the activity of both radionuclides in the river water, based on the relation between the amount of sludge generated and the flow of the river water treated in the plant. Based on this estimation, it is possible avoid the use of time-consuming methods.

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“…Several methods have been proposed for elemental determination in soil and sediments samples using different analytical techniques, among others atomic fluorescence (AFS), X-ray fluorescence spectrometry (XRF), neutron activation analysis (NAA), atomic absorption spectrometry (AAS), inductively coupled plasma optical emission spectrometry (ICP OES), or inductively coupled plasma mass spectrometry (ICP-MS) (Soodan et al 2014;Roje 2011;Melaku et al 2005). However, ICP-MS is one of the most widely used, apart from its multi-elemental capability this technique offers a high sensitivity, wide dynamic range, isotope ratio information, and the possibility of sample introduction using alternative devices such as electrothermal vaporization (ETV) and laser ablation (LA) (Krishna et al 2012).…”

Section: Introductionmentioning

confidence: 99%

“…The procedure for soil and sediment digestion is mainly carried out by alkaline fusion (Uchida et al 2005), acid digestion using mineral acid and heating with a hot plate (Kelepertzis 2014), or applying a microwave-assisted digestion (Marin et al 2008;Roje 2011;Melaku et al 2005). The US Environmental Protection Agency (EPA) has published the methods EPA 3050, 3051, 3051a, and 3052 for acid digestion of soil, sediments, and sludge samples for analysis by AAS, ICP OES, and ICP-MS techniques (Silva et al 2014).…”

Section: Introductionmentioning

confidence: 99%

Determination of metals in Brazilian soils by inductively coupled plasma mass spectrometry

Carvalho

Santos

Silva

et al. 2015

Environ Monit Assess

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The concentration of metals in Brazilian soil under no-tillage (NT) and an area under native vegetation (NV) was determined by inductively coupled plasma mass spectrometry. The applied method was based on microwave-assisted acid digestion using HNO3, HCl, H2O2, and HF. The accuracy of the method was evaluated by analyzing two certified reference materials (BCR-142 and RS-3). The relative standard deviation for all target elements was below 8% indicating an adequate precision and the limit of detection ranged from 0.03 μg g(-1) (Cd) to 24.0 μg g(-1) (Fe). The concentrations of Al, As, Ba, Cd, Cu, Fe, Mg, Mn, Ni, Pb, Sr, and Zn in the different layers (0-10, 10-20, 20-40, and 40-60 cm) were determined in two types of soils, located in Paraná State in Brazil. The soil layers analysis revealed a different behavior of metals concentrations in soil samples under NT and NV. The obtained results showed a clear impact of anthropogenic action with respect to specific metals due to many years of uncontrolled application rates of limestone and phosphate fertilizers.

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Fast method of multi-elemental analysis of stream sediment samples by inductively coupled plasma-mass spectrometry (ICP-MS) with prior single-step microwave-assisted digestion

Cited by 10 publications

References 11 publications

Evaluation of Analytical Methods for Lead (Pb) (USEPA 3051) and Zinc (Zn) (HR-CS AAS) in Sediments

Evaluation of Analytical Methods for Lead (Pb) (USEPA 3051) and Zinc (Zn) (HR-CS AAS) in Sediments

Determination of artificial beta-emitters in sludge samples

Determination of metals in Brazilian soils by inductively coupled plasma mass spectrometry

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