Preparo de amostras de combustíveis fósseis por piroidrólise para a determinação de flúor e cloro

Antes, Fabiane Goldschmidt; Duarte, Fábio A.; Flores, Éder Lisandro Moraes; Paniz, José Neri Gottfried; Flores, Érico M.M.; Dressler, Valderi L.

doi:10.1590/s0100-40422010000500024

Cited by 27 publications

(18 citation statements)

References 13 publications

(33 reference statements)

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“…7,24,33,36 However, for other samples, like coal and petroleum coke, halogens are released without any auxiliary reagent. 19,33,38 Figure 2. Influence of Na 2 CO 3 /NaHCO 3 solution concentration used for collection of Br (¢) and I (¢); error bars are the standard deviations, n = 5.…”

Section: Influence Of Accelerator On Analyte Recoveriesmentioning

confidence: 99%

“…Pyrohydrolysis is a simple alternative for decomposition of organic 7,19,31,33 and inorganic [34][35][36] materials when halogens determination is intended. The main advantages are the possibility of matrix separation and the use of a diluted alkaline solution for analytes absorbing.…”

Section: Introductionmentioning

confidence: 99%

“…Therefore the time necessary for pyrohydrolysis can change according to sample matrix, analyte concentration and also the characteristics of the pyrohydrolysis system employed. 17,19,32,37,39 In comparison with other sample preparation techniques 10,20,25 for subsequent halogens determination, the pyrohydrolysis method proposed in this work can be considered relatively fast because up to 5 samples can be decomposed in 1 h. …”

mentioning

confidence: 99%

“…18 It is worth citing that ICP-MS is a powerful technique for halogens determination (except for fluorine) due to the high sensitivity observed. 19 However, the high salt content in mineral supplements used for animal nutrition causes serious interferences and, therefore, matrix separation is necessary. 20,21 Sample preparation is usually the bottleneck in halogen determination by ICP-MS, due to memory effects caused by high volatility of halogens in acidic solutions.…”

mentioning

confidence: 99%

“…20,21 Sample preparation is usually the bottleneck in halogen determination by ICP-MS, due to memory effects caused by high volatility of halogens in acidic solutions. [22][23][24] Therefore, alkaline fusion, 20 dilution or dispersion in alkaline solution, distillation (for fluorine), combustion in bombs, 25 microwave-induced combustion (MIC) 9,26-29 and pyrohydrolysis 7,17,[30][31][32] are used for sample preparation.Pyrohydrolysis is a simple alternative for decomposition of organic 7,19,31,33 and inorganic 34-36 materials when halogens determination is intended. The main advantages are the possibility of matrix separation and the use of a diluted alkaline solution for analytes absorbing.…”

mentioning

confidence: 99%

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Determination of bromine, fluorine and iodine in mineral supplements using pyrohydrolysis for sample preparation

Taflik

Duarte

Flores

et al. 2012

J. Braz. Chem. Soc.

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Neste trabalho foi utilizada a piroidrólise para a decomposição de suplemento mineral utilizado na nutrição animal, para a posterior determinação de F, Br e I. Flúor foi determinado por potenciometria utilizando eletrodo íon-seletivo para fluoreto, enquanto que Br e I foram determinados por espectrometria de massa com plasma indutivamente acoplado. Os principais parâmetros que influenciam a piroidrólise foram investigados e, após a devida avaliação dos mesmos, foram fixadas as seguintes condições: a temperatura do reator em 1000 °C durante 10 min; a proporção entre a massa de amostra e a massa de acelerador em 1 + 5 e a vazão do gás carreador em 200 mL min -1 . A exatidão do método foi avaliada usando teste de recuperação do analito e análise de materiais de referência certificados de rocha fosfática e de solo. O método foi aplicado para análise de suplemento mineral. Os limites de quantificação foram de 16, 0,3 e 0,07 µg g -1 para F, Br e I, respectivamente. Assim, usando-se um método relativamente simples e de baixo custo é possível a decomposição de até 5 amostras por hora. Portanto, a piroidrólise pode ser usada como um método de rotina para o preparo de amostra de suplemento mineral para a determinação de F, Br e I.Pyrohydrolysis was employed for mineral supplements decomposition prior to F, Br and I determination. Fluoride determination was carried out by potentiometry using a fluoride-ion selective electrode, whereas Br and I were determined by inductively coupled plasma mass spectrometry. The main parameters that influence on pyrohydrolysis were investigated. After evaluation, the following conditions were established: reactor temperature of 1000 °C during 10 min; sample plus accelerator mass ratio of 1 + 5 and carrier gas (air) flow rate of 200 mL min -1 . The accuracy of the proposed method was evaluated by analyte recovery tests and analysis of certified reference materials of phosphate rock and soil. Commercial mineral supplement samples were analyzed. The limits of quantification were 16, 0.3 and 0.07 µg g -1 for F, Br and I, respectively. By using a relatively simple and low cost pyrohydrolysis system up to 5 samples can be processed per hour. The developed sample preparation procedure can be routinely employed for F, Br and I determination in mineral supplements. Keywords: pyrohydrolysis, halogens determination, mineral supplement IntroductionSeveral elements are essential for animals growing and breeding. Those elements required in high amounts are called macronutrients (Ca, Cl, K, P, Mg, Na, and S) and those elements required in low concentrations are called micronutrients (Co, Cu, Fe, I, Mn, Mo, Se, Zn, and eventually Cr and F are included in this group). 1 The main functions of essential elements in the organism are associated to the structural composition of body and enzymatic and hormonal processes.Although F usually increases the strength of bones and teeth, this element is generally not considered as essential. 1 Fluorine is usually present as a contaminant since it is Taflik et al. 489 ...

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Section: Influence Of Accelerator On Analyte Recoveriesmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

mentioning

confidence: 99%

mentioning

confidence: 99%

mentioning

confidence: 99%

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Determination of bromine, fluorine and iodine in mineral supplements using pyrohydrolysis for sample preparation

Taflik

Duarte

Flores

et al. 2012

J. Braz. Chem. Soc.

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Challenges and trends for halogen determination by inductively coupled plasma mass spectrometry: A review

Flores

Mello

Krzyzaniak

et al. 2020

Rapid Comm Mass Spectrometry

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Rationale In this review, works published in the past 25 years for fluorine, chlorine, bromine, and iodine determination in several matrices by inductively coupled plasma mass spectrometry (ICP‐MS) were covered. Usually, the determination of halogens has been performed by ICP‐MS using a previous sample preparation step or, more recently, by direct analysis of solid or liquid samples. Methods Methods based on combustion, extraction, pyrohydrolysis, sample dilution in organic or aqueous medium, and wet digestion, among others, are discussed. Moreover, the recent applications of methods based on laser ablation (LA) and electrothermal vaporization (ETV) coupled to ICP‐MS are discussed. Results The main challenge for methods using sample preparation has been to obtain a final solution compatible with ICP‐MS, as well as to overcome problems related to analyte losses and contamination. Interferences due to the presence of dissolved organic compounds in solution, enhancement or suppression of ionization of analytes, and related matrix effects have been of concern when using ICP‐MS. For the determination of halogens by ICP‐MS using LA and ETV systems, some limitations related to the difficulty of calibration are pointed out, impairing the widespread use of this approach. Conclusions A critical view is presented for further halogen determination by ICP‐MS, mainly for matrices considered difficult to digest using conventional protocols.

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Analytical methods for the determination of halogens in bioanalytical sciences: a review

et al. 2013

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Fluorine, chlorine, bromine, and iodine have been studied in biological samples and other related matrices owing to the need to understand the biochemical effects in living organisms. In this review, the works published in last 20 years are covered, and the main topics related to sample preparation methods and analytical techniques commonly used for fluorine, chlorine, bromine, and iodine determination in biological samples, food, drugs, and plants used as food or with medical applications are discussed. The commonest sample preparation methods, as extraction and decomposition using combustion and pyrohydrolysis, are reviewed, as well as spectrometric and electroanalytical techniques, spectrophotometry, total reflection X-ray fluorescence, neutron activation analysis, and separation systems using chromatography and electrophoresis. On this aspect, the main analytical challenges and drawbacks are highlighted. A discussion related to the availability of certified reference materials for evaluation of accuracy is also included, as well as a discussion of the official methods used as references for the determination of halogens in the samples covered in this review.

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Preparo de amostras de combustíveis fósseis por piroidrólise para a determinação de flúor e cloro

Cited by 27 publications

References 13 publications

Determination of bromine, fluorine and iodine in mineral supplements using pyrohydrolysis for sample preparation

Determination of bromine, fluorine and iodine in mineral supplements using pyrohydrolysis for sample preparation

Challenges and trends for halogen determination by inductively coupled plasma mass spectrometry: A review

Analytical methods for the determination of halogens in bioanalytical sciences: a review

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