Chromium determination in pharmaceutical grade barium sulfate by solid sampling electrothermal atomic absorption spectrometry with Zeeman-effect background correction

Bolzan, Rodrigo Cordeiro; Rodrigues, Luiz Frederico; Mattos, Julio Cezar Paz de; Dressler, Valderi L.; Flores, Érico M.M.

doi:10.1016/j.talanta.2007.05.032

Cited by 23 publications

(16 citation statements)

References 33 publications

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“…In a previous work it was found that 64% of the barium sulfate mass remained in the platform even with pyrolysis temperature of 1500 o C and the residual matrix vaporized concomitantly with the analyte during atomization step. 30 This is compatible with the thermal decomposition of BaSO 4 yielding BaO, SO 2 and O 2 , at temperatures prior the melting point of barium sulfate (1580 o C). 31,32 Background signals could be originated by molecules as C n S m (with n>m) formed in the gas phase at high temperatures, which yields diffuse bands from 187 to 230 nm region.…”

Section: Pyrolysis and Atomization Profiles For Arsenic In Barium Sulsupporting

confidence: 75%

“…The addition of hydrogen has been proposed for pre-reduction of Pd modifier on the surface of graphite tube yielding metallic Pd in order to increase its efficiency. 34 Contrarily to Cr determination, in this matrix 30 the use of chemical modifier and hydrogen addition were necessary due to the high matrix interference observed in the selected wavelength for As. Analytical signals for As in BaSO 4 with palladium and also hydrogen addition during pyrolysis step showed better profile and lower BG signals using both correction systems, specially for Z-SoS-ET AAS ( Figures 1C and 1D).…”

Section: Pyrolysis and Atomization Profiles For Arsenic In Barium Sulmentioning

confidence: 99%

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Arsenic determination in pharmaceutical grade barium sulfate using direct solid sampling electrothermal atomic absorption spectrometry

Bolzan¹,

Moraes²,

Mattos³

et al. 2010

J. Braz. Chem. Soc.

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Um método para determinação de arsênio em BaSO 4 por espectrometria de absorção atômica com aquecimento eletrotérmico e introdução de amostras sólidas (SoS-ET AAS) é descrito. Foram avaliados dois sistemas de correção de fundo (BG), deutério e efeito Zeeman (Z). Com o uso combinado de hidrogênio e Pd o BG foi diminuído. Resultados exatos e precisos foram obtidos usando Z-SoS-ET AAS. O desvio padrão relativo usando Z-SoS-ET AAS foi menor que 9,5%. O limite de detecção foi 0,005 mg g -1 e a massa característica foi 25,4 pg. Os resultados foram comparados com os obtidos usando o método de preparo de amostras sugerido pela Farmacopeia Europeia, com determinação usando espectrometria de emissão ótica e espectrometria de massas, ambos com plasma indutivamente acoplado, porém os resultados foram cerca de 20% menores. Vantagens como simplicidade, elevada frequência de determinações e boa exatidão foram obtidos em comparação com o método descrito na farmacopeia.A method for arsenic determination in pharmaceutical grade BaSO 4 by solid sampling electrothermal atomic absorption spectrometry (SoS-ET AAS) is described. Two background (BG) correction systems, deuterium and Zeeman-effect (Z), were evaluated. Background was decreased by using hydrogen combined with Pd. Accurate and precise results were obtained using Z-SoS-ET AAS. Relative standard deviation using Z-SoS-ET AAS was lower than 9.5%. Limit of detection was 0.005 mg g -1 and characteristic mass was 25.4 pg. Results were also compared with those obtained using the preparation method suggested by European Pharmacopoeia for BaSO 4 followed by determination using inductively coupled plasma optical emission spectrometry and inductively coupled plasma mass spectrometry. Results were around 20% lower than results obtained using the proposed method. Some advantages as simplicity, higher sample throughput were found when compared with the official method currently described in pharmacopoeia.

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Section: Pyrolysis and Atomization Profiles For Arsenic In Barium Sulsupporting

confidence: 75%

Section: Pyrolysis and Atomization Profiles For Arsenic In Barium Sulmentioning

confidence: 99%

Arsenic determination in pharmaceutical grade barium sulfate using direct solid sampling electrothermal atomic absorption spectrometry

Bolzan¹,

Moraes²,

Mattos³

et al. 2010

J. Braz. Chem. Soc.

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“…This result is consistent with previous reports in the literature 7,14,23,24 for the determination of Cr in several matrices by GF AAS. Thus, matrix modifiers were not used in further experiments.…”

Section: Chemical Modifiersupporting

confidence: 93%

“…Graphite furnace AAS technique is applied extensively to the determination of Cr in various matrices, 7,13,14,[23][24][25] however there are few studies on the determination of Cr in crude oil. Stigter et al 7 determined Cr in crude oil after dilution with toluene and acetic acid; Burguera et al 25 determined it after emulsion formation; Dittert et al 14 determined Fe and Cr simultaneously by HR-CS GF AAS (high-resolution continuum source graphite furnace atomic absorption spectrometry), but they did not present the properties of the samples used and depending on the API degree, the procedure cannot be adequate.…”

Section: Introductionmentioning

confidence: 99%

“…Some procedures related to sample preparation for metal determination in crude oil can be used, such as acid digestion, 8 dilution with organic solvents, 7,26,27 emulsion or microemulsion formation 22,23,28,29 and direct sampling (DS) using an automatic solid sampling accessory. 14,[30][31][32] Acid digestion is time consuming, presents risks of losses of analyte and sample contamination, and also requires the use of corrosive and hazardous reagents; thus it is the least suitable for routine work, although it allows instrument calibration with aqueous calibration solutions.…”

Section: Introductionmentioning

confidence: 99%

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Comparison of different pre-treatment procedures for the determination of chromium in crude oil samples by GF AAS

Pessoa

Lyra

Castro

et al. 2012

J. Braz. Chem. Soc.

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No presente estudo, três procedimentos de pré-tratamento e determinação de Cr por GF AAS foram desenvolvidos e comparados: diluição da amostra com tolueno, formação de emulsão e amostragem direta do petróleo. Os limites de detecção para os procedimentos desenvolvidos foram 1,9 ng g -1 para a diluição da amostra com tolueno, 2,8 ng g -1 para a formação de emulsão e 0,73 ng g -1 para a amostragem direta. A exatidão dos três procedimentos foi avaliada analisando-se o material NIST1085b e por testes de recuperação. Em todos os procedimentos foram obtidos altos valores de recuperação e boa concordância entre os teores determinados e os teores certificados. No entanto, os resultados indicam que a diluição da amostra com tolueno não é recomendada para amostras com grau API abaixo de 15. Os outros dois procedimentos mostraram o mesmo desempenho para as amostras com diferentes graus API (8-38), mas a amostragem direta apresentou melhor sensibilidade além de minimizar as chances de perdas do analito ou contaminação.In the present study three pre-treatment procedures were developed and compared following Cr determination by GF AAS: sample dilution with toluene, emulsion formation and direct sampling of crude oil. The limits of detection for the developed procedures were 1.9 ng g -1 for sample dilution with toluene, 2.8 ng g -1 for emulsion formation and 0.73 ng g -1 for direct sampling. The accuracy of the three procedures was assessed by analysis of NIST1085b and recovery tests. High recoveries and good agreement between found and certified values were obtained in all cases. However, results indicate that sample dilution with toluene is not recommended for samples below 15ºAPI. The other two procedures showed the same performance for the samples with different API degrees (8 to 38), but the direct sampling showed better sensitivity besides minimizing the chances of analyte losses or contamination.

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Determination of elemental impurities in pharmaceutical products and related matrices by ICP-based methods: a review

et al. 2016

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Interest in the determination of elemental impurities in pharmaceuticals has increased in recent years because of changes in regulatory requirements and the need for changing or updating the current limit tests recommended in pharmacopeias. Inductively coupled plasma (ICP) optical emission spectrometry and ICP mass spectrometry are suitable alternatives to perform multielemental analysis for this purpose. The main advantages and limitations of these techniques are described, covering the applications reported in the literature in the last 10 years mainly for active pharmaceutical ingredients, raw materials, and pharmaceutical dosage forms. Strategies used for sample preparation, including dissolution in aqueous or organic solvents, extraction, wet digestion and combustion methods are described, as well as direct solid analysis and ICP-based systems applied for speciation analysis. Interferences observed during the analysis of pharmaceutical products using ICP-based methods are discussed. Methods currently recommended by pharmacopeias for elemental impurities are also covered, showing that the use of ICP-based methods could be considered as a trend in the determination of these impurities in pharmaceuticals. However, the development of a general method that is accurate for all elemental impurities and the establishment of an official method are still challenges. In this regard, the main drawbacks and suitable alternatives are discussed.

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Chromium determination in pharmaceutical grade barium sulfate by solid sampling electrothermal atomic absorption spectrometry with Zeeman-effect background correction

Cited by 23 publications

References 33 publications

Arsenic determination in pharmaceutical grade barium sulfate using direct solid sampling electrothermal atomic absorption spectrometry

Arsenic determination in pharmaceutical grade barium sulfate using direct solid sampling electrothermal atomic absorption spectrometry

Comparison of different pre-treatment procedures for the determination of chromium in crude oil samples by GF AAS

Determination of elemental impurities in pharmaceutical products and related matrices by ICP-based methods: a review

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