A direct solid sampling electrothermal atomic absorption spectrometric method for determination of trace elements in zirconium dioxide

Kriváň, V.; Janickova, Petra

doi:10.1007/s00216-005-3306-1

Cited by 13 publications

(8 citation statements)

References 23 publications

Supporting

Mentioning

Contrasting

Order By: Relevance

“…33,34,36,[40][41][42] Sometimes, solid reference materials can be required or even it could be necessary to add the standard solution onto the residual matrix remaining from the previous sample run. 47 One of the main requirements for the development of a calibration method using aqueous standard solutions is that when analyzing solid samples the matrix effect on the absorbance signal is negligible.…”

Section: Analysis Of Carbon Nanotube Samplesmentioning

confidence: 99%

“…23 On the other hand, the direct analysis of solid samples has been proposed as an alternative in atomic absorption spectrometry. [27][28][29][30] Direct solid sampling electrothermal atomic absorption spectrometry (DSS-ET AAS) has proven to be a highly worthwhile method for the analysis of several very difficult matrices to digest, as aluminum oxide, 31 silicon carbide, 32 silicon nitride, 33 sand, 34 alumina based catalysts, 35 zirconium dioxide, 36 boron nitride, 37 polymers 38 and graphite. 32 Several advantages of DSS-ET AAS have been reported as the low risk of contamination and relatively small sample mass requirement.…”

Section: Introductionmentioning

confidence: 99%

See 1 more Smart Citation

Determination of metal impurities in carbon nanotubes by direct solid sampling electrothermal atomic absorption spectrometry

Mello¹,

Rodrigues²,

Nunes³

et al. 2011

J. Braz. Chem. Soc.

View full text Add to dashboard Cite

soluções aquosas e massa máxima de amostra. Para comparação dos resultados as amostras foram analisadas por espectrometria de massa com plasma indutivamente acoplado (ICP-MS) e espectrometria de emissão óptica com plasma indutivamente acoplado (ICP OES) após decomposição por via úmida em sistema de alta pressão assistida por micro-ondas e também por combustão iniciada por micro-ondas. Não foram observadas diferenças significativas entre os resultados obtidos pelo método proposto e pelas outras técnicas. A exatidão também foi avaliada por comparação com resultados de análise por ativação neutrônica (NAA). A calibração foi possível com soluções de referência aquosas. Os sinais de fundo foram sempre inferiores a 0,02 (altura de pico) e o uso de modificador químico não foi necessário. O método proposto possibilitou a determinação de todos os analitos, com menores limites de detecção quando comparados com as outras técnicas.Metal impurities (Al, Cd, Co, Cr, Cu, Mg, Mn and Pb) were determined in carbon nanotubes (CNTs) by direct solid sampling electrothermal atomic absorption spectrometry (DSS-ET AAS, deuterium lamp background corrector). Parameters as pyrolysis and atomization temperatures, use of Pd as chemical modifier, feasibility of calibration using aqueous standard solutions and maximum sample mass were investigated. Results obtained by the proposed method were compared with those obtained by neutron activation analysis (NAA) and also by inductively coupled plasma mass spectrometry (ICP-MS) and inductively coupled plasma optical emission spectrometry (ICP OES) after high-pressure microwave assisted wet digestion and microwave-induced combustion methods. No significant differences were observed between the results obtained by DSS-ET AAS, ICP-MS and ICP OES after both digestion methods and also by NAA. Calibration was performed using aqueous standards. Background signals were always lower than 0.02 (peak height) and no chemical modifier was used. The proposed method allowed the determination of all elements in CNTs with lower limits of detection in comparison with other techniques.Keywords: carbon nanotubes, metal impurities, solid sampling, electrothermal atomic absorption spectrometry IntroductionSince the advent of nanotechnology the development of new materials with a wide range of special properties has been performed for very different applications in almost all technological fields. With the discovery of carbon nanotubes (CNTs) by Iijima, 1 this new class of nanomaterials provided unique chemical, mechanical and electronic properties. In recent years, carbon nanotubes have received a growing interest in several fields as materials industry, electronics, medicine and also in analytical applications. [2][3][4][5][6][7] Carbon nanotubes can be described as a kind of graphite structure which is based on benzene-type hexagonal rings of carbon atoms, rolled up in a nanoscale tube (diameter ranging from a few tenths to tens of nanometers). This nanomaterial can be defined as a single-wall carbon nanotube (SWCNT) ...

show abstract

Section: Analysis Of Carbon Nanotube Samplesmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Determination of metal impurities in carbon nanotubes by direct solid sampling electrothermal atomic absorption spectrometry

Mello¹,

Rodrigues²,

Nunes³

et al. 2011

J. Braz. Chem. Soc.

View full text Add to dashboard Cite

show abstract

“…Addition of graphite has been proposed in direct solid sampling-graphite furnace atomic absorption spectrometry in order to allow sensitivities more close to those using reference solutions. 32 In this work, tests were performed by mixing samples with 30 mg of high purity graphite powder and pressed as pellets. With this condition, results for characteristic mass were more similar between samples and reference solution added to graphite pellets used for calibration and graphite addition was used for further oxygen flow-rate, flame stoichiometry, calibration and sample mass evaluation.…”

Section: Optimization Of Operating Conditions For Mic-ff-aasmentioning

confidence: 99%

Determination of Cd in blood by microwave-induced combustion coupled to flame furnace atomic absorption spectrometry

Hoehne¹,

Bartz²,

Bizzi³

et al. 2010

J. Braz. Chem. Soc.

View full text Add to dashboard Cite

Um sistema de combustão iniciada por microondas foi acoplado a um espectrômetro de absorção atômica com atomização em tubo metálico aquecido com chama (FF) do tipo ar-acetileno para a determinação de cádmio em sangue. Amostras de sangue liofilizado foram preparadas como comprimidos, posicionadas em um suporte de quartzo e introduzidas em uma câmara de vidro empregada para a etapa de combustão. A câmara foi acoplada ao tubo metálico usando tubos de politetrafluoroetileno e de quartzo. A ignição foi iniciada por irradiação microondas usando solução de nitrato de amônio adicionada em papel previamente descontaminado. Oxigênio foi usado na etapa de combustão e para o transporte dos produtos gerados até o tubo aquecido. Grafite em pó de alta pureza foi misturada com as amostras antes do preparo dos comprimidos. O volume da solução de NH 4 NO 3 , a vazão de oxigênio, a estequiometria da chama, o tipo de suporte e a quantidade de massa de amostra foram avaliados. A calibração foi possível usando solução de referência adicionada a comprimidos de grafite de alta pureza, não sendo necessário o uso de material de referência certificado (CRM). Foi possível a combustão de até 56 mg de amostra, permitindo a obtenção de limite de quantificação de 0,018 µg g -1 e massa característica de 50 pg de Cd. Os valores dos brancos foram baixos (absorbância integrada menor que 0,01 s). Os resultados foram considerados satisfatórios com respeito à exatidão (concordância com valores de CRMs entre 95 e 99%) e à precisão (coeficiente de variação < 12%). Até 15 determinações podem ser feitas por hora incluindo a etapa de pesagem.Microwave-induced combustion system was coupled to a metallic flame furnace (FF) atomic absorption spectrometer and applied for cadmium determination in blood. Lyophilized blood samples were prepared as pellets, positioned on a quartz holder and introduced into a glass chamber used for the combustion step. The glass chamber was coupled to the metallic flame furnace by using polytetrafluoroethylene and quartz tubes. Ignition was performed by microwave radiation using ammonium nitrate solution added to a small piece of previously cleaned paper. Oxygen was used to assist the sample combustion and also to transport combustion products up to the FF heated by an air/acetylene flame. High purity graphite powder was mixed with samples before pellets preparation. The volume of NH 4 NO 3 solution, oxygen flow-rate, flame stoichiometry, sample holder type and the sample mass range were evaluated. Calibration step was feasible using adsorbed reference solution in pelletized high purity graphite avoiding the use of certified reference material (CRM). Sample masses up to 56 mg could be used allowing quantification limit of 0.018 µg g -1 and characteristic mass of 50 pg Cd. Low values for blanks were obtained (integrated absorbance lower than 0.01 s) and results were considered satisfactory regarding to both accuracy (agreement with results using CRMs between 95 to 99%), and precision (relative standard deviation < 12%). Up to 15 de...

show abstract

“…For the determination of trace metallic constituents, they either have to be separated physically from the trace metals using the d.c. arc carrier distillation technique (1)(2)(3)(4)(5)(6) or by chemical separation, followed by ICP-AES analysis of the raffinate (7)(8)(9)(10)(11)(12)(13)(14)(15). Different approaches were found in the literature for the determination of analytes in Zr matrices (28)(29).…”

Section: Introductionmentioning

confidence: 99%

Determination of Common Analytes at Trace Levels in Zr Matrix by ICP-AES Without Chemical/Physical Separation

Sengupta¹

2013

At.Spectrosc.

View full text Add to dashboard Cite

Chemical (ICP-AES) or physical (d.c. arc carrier distillation technique) separation of the major matrix, followed by the determination of trace metallic impurities in the raffinate, is a well accepted protocol in the nuclear industries to avoid spectral interferences from emissionrich matrices such as U, Pu, Zr, Th, etc. With ICP-AES analysis, the RSD is better (less than 5%), separation is time-consuming, involves handling of the materials which increases the chances of contamination, while the precision of the d.c. arc technique is 15-25%. Thus, there is a need to have an ICP-AES-based methodology where the analytes can be determined in a nuclear matrix at trace levels without requiring chemical separation. In this paper, an attempt was made to develop a method for the determination of trace constituents in a Zr matrix without separation by using the flexibility of a charge coupled device (CCD) detector for choosing additional interference-free analytical lines for Mn,

show abstract

A direct solid sampling electrothermal atomic absorption spectrometric method for determination of trace elements in zirconium dioxide

Cited by 13 publications

References 23 publications

Determination of metal impurities in carbon nanotubes by direct solid sampling electrothermal atomic absorption spectrometry

Determination of metal impurities in carbon nanotubes by direct solid sampling electrothermal atomic absorption spectrometry

Determination of Cd in blood by microwave-induced combustion coupled to flame furnace atomic absorption spectrometry

Determination of Common Analytes at Trace Levels in Zr Matrix by ICP-AES Without Chemical/Physical Separation

Contact Info

Product

Resources

About