Spectrometric methods for the determination of chlorine in crude oil and petroleum derivatives — A review

Doyle, Adriana; Saavedra, A.; Tristão, Maria Luiza B.; Mendes, Luiz A.N.; Aucélio, Ricardo Q.

doi:10.1016/j.sab.2013.06.003

Cited by 27 publications

(19 citation statements)

References 29 publications

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“…Although found in trace amounts chlorine is very deleterious since during the processing of crude oil it generates hydrochloric acid which is strongly corrosive and can cause serious damage to the components of the equipments. [1][2][3][4] Chlorine determination in crude oil is not an easy task due to the complexity of the sample and the possibility of analyte lost during the treatment procedures prior the analysis. The determination of chlorine has been performed following official methods of the American Society for Testing and Materials, ASTM D3230, 5 ASTM D6470 6 and ASTM D4929, 7 and the US Environmental Protection Agency, method EPA 9075.…”

Section: Introductionmentioning

confidence: 99%

Determination of Chlorine in Crude Oil Emulsified via the MgCl Molecule by HR‑CS MAS

Oliveira¹,

Medeiros²,

Silva³

et al. 2017

J. Braz. Chem. Soc.

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A method for chlorine determination in crude oil samples, through the formation of MgCl molecule, by high-resolution continuum source graphite furnace molecular absorption spectrometry (HR-CS GF MAS) was developed and is described in this paper. The use of this molecule for chlorine determination in crude oil has not been reported up to now. Measures were carried out at the wavelength 377.010 nm and the samples were submitted to a simple treatment as emulsion, whose composition was optimized applying a simplex-centroid experimental design. Magnesium was used as molecule forming agent at the concentration of 10 g L -1 , at least 500 times higher than the concentration of chlorine. This excess is required to ensure the molecule formation of all content of Cl present in the sample. Chemical modifier Pd was used and improved greatly the signal intensities. Optimized pyrolysis and vaporization temperatures, applied for determination, were 800 and 2300 °C, respectively. Accuracy was evaluated through analysis of certified reference materials, NIST 1848 and NIST 1634c, and addition and recovery tests with recoveries between 92 and 117%. Limits of detection and quantification were 3.0 and 9.0 µg g -1 , respectively. The method was applied to eight crude oil samples.

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Section: Introductionmentioning

confidence: 99%

Determination of Chlorine in Crude Oil Emulsified via the MgCl Molecule by HR‑CS MAS

Oliveira¹,

Medeiros²,

Silva³

et al. 2017

J. Braz. Chem. Soc.

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“…This control is fundamental, as the maximum content of salts, expressed as the mass of sodium chloride in mg dissolved in 1 kg of crude oil, is 570 mg kg À1 for the production step; in refineries, the content of salts should be lower than 5 mg kg À1 [4]. In parallel, the high temperatures of distillation towers can promote the hydrolysis of chloride, generating hydrochloric acid as a final product, which is one of the main causes of corrosive processes in crude oil refineries [10][11][12][13][14].…”

Section: Introductionmentioning

confidence: 99%

“…Among the salts present in crude oil, sodium, calcium, magnesium, strontium and iron chlorides are the most common and, along with carbonate and sulphate salts, are the main cause of corrosion and encrustation [8,[12][13][14]. The counterions (Na, Ca, Mg, Sr and Fe) associated with chloride can be extracted in the aqueous phase of crude oil using the standard ASTM D 6470-99 test method [15].…”

Section: Introductionmentioning

confidence: 99%

“…However, no available study mentions the use of this technique for the monitoring of chloride via the determination of its main counterions in aqueous crude oil extracts. Most studies emphasise the determination of metals and nonmetals either directly in crude oil and its derivatives [18][19][20][21] or after microwave digestion [6,7,10,14,22]. However, destabilisation issues and the extinction of plasma, which are associated with low sensitivity, are frequent occurrences when samples with a high carbon content (e.g., crude oil) are directly introduced into ICP-OES, affecting the precision and accuracy of the results.…”

Section: Introductionmentioning

confidence: 99%

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Evaluation and determination of chloride in crude oil based on the counterions Na, Ca, Mg, Sr and Fe, quantified via ICP-OES in the crude oil aqueous extract

Souza

Ribeiro

Carneiro

et al. 2015

Fuel

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h i g h l i g h t sChloride salts contained in crude oil can cause corrosion and encrustation in distillation towers. Chloride concentrations can be obtained via ICP-OES through the analysis of its counterions. The accuracy of the procedure was confirmed through comparison with the results of FAAS. The modified standard test method of ASTM D 6470-99 extraction was compared with microwave-assisted acid digestion. The study demonstrated that Na, Ca, Mg, Sr and Fe were mainly associated with chloride. a b s t r a c tOf the salts present in crude oil, sodium, calcium, magnesium, strontium and iron chlorides are the most abundant and are considered the main cause of corrosion in crude oil refineries. Therefore, the objective of this study was to quantify the main chloride counterions (Na, Ca, Mg, Sr and Fe) using inductively coupled plasma-optical emission spectrometry (ICP-OES) after hot solvent extraction (modified ASTM D 6470-99). The procedure developed in this work allowed samples with different°API values (17.4-30.2) originating from the post-salt to be studied. Under the operational conditions of ICP-OES, robust plasma (Mg II/Mg I > 10 for the axial and radial configurations) was obtained based on evaluation of the ratio of the Mg II/Mg I intensities. Furthermore, yttrium was used as an internal standard, resulting in as little interference with the analytical signal as possible. This procedure achieved detection limits on the order of 0.99 mg L À1 , 0.025 mg L À1 , 0.33 lg L À1 , 0.06 ng L À1 and 0.26 lg L À1 for Na, Ca, Mg, Sr and Fe, respectively. The accuracy of the procedure was confirmed through addition/recovery tests (91-120%) and through comparison with the results obtained with flame atomic absorption spectrometry (FAAS). The modified standard test method of ASTM D 6470-99 extraction was compared with microwaveassisted acid digestion and was found to achieve extractions higher than 92.44% for Na and 81.06% for Sr from two of the analysed extracts. Finally, the chloride concentrations obtained via potentiometric titration and ICP-OES (through the analysis of chloride with its counterions) in the aqueous extract indicated a high correlation between Na, Ca, Mg, Sr and Fe and chloride (105.10%, 99.33% and 102.12% for the evaluated samples).

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“…Ele é utilizado em muitas áreas diferentes, como a produção de solventes clorados e outros reagentes, purificação de água, produção de plásticos, e indústria de papel e celulose [181]. Por isso, o controle do conteúdo deste elemento é necessário em nível traço em uma grande variedade de amostras [182][183][184][185][186][187][188][189].…”

Section: Introductionunclassified

Desenvolvimento de procedimentos analíticos para a determinação de não-metais via moléculas diatômicas por espectrometria de absorção molecular de alta resolução com fonte contínua

Nakadi¹

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iii Dedico esta teseA meus pais, Ruth e Ivo, os quais me acompanham e incentivam o meu crescimento. Tudo o que me compõe é fruto de sua dedicação e carinho. Amo vocês.À minha irmã, Cintia, cuja companhia sempre me trouxe muita alegria, apesar do oposto não ser verdadeiro. Muito obrigado. Tabela 3. Determinação de bromo em amostra de teclas submetida à digestão ácida (DA) com posterior dissolução em NH4OH ou à extração Soxhlet (ES) com tolueno, com adição de bromo como NaBr. Intervalo de confiança de 95 % (n = 3)…………... 36 Tabela 4. Programa de temperatura utilizado para a determinação de enxofre em suspensão de carvão e cinzas por HR CS GFMAS……………………………………. 42 Tabela 5. Figuras de mérito da determinação de enxofre em carvão e cinzas via molécula CS por HR CS MAS………………………………………………………… 47 Tabela 6. Determinação de enxofre em suspensão de carvão e cinzas (CRMs) através da molécula de CS por HR CS GFMAS. A incerteza é expressa como intervalo de confiança de 95 % (n = 3)……………………………………………………………… 49 Tabela 7. Parâmetros utilizados para determinar enxofre via molécula de CS por HR CS MAS………………………………………………………………………………... 54 Tabela 8. Figuras de mérito do MEA e da ADD com avaliação do sinal da molécula CS determinada pela soma de 3 pixels (PC ± 1). Os LD e LQ apresentados fora do parêntesis foram calculados por, respectivamente, três e dez vezes o desvio padrão do branco (n = 10) dividido pela inclinação da curva de calibração. Os LD e LQ dos métodos estão dentro do parêntesis, considerando a diluição da amostra (aproximadamente 50 vezes para MEA) e massa de amostra (aproximadamente 3 mg para ADD)……………………………………………………………………………... 67 Tabela 9. Comparação entre a concentração de enxofre das amostras de referência determinadas pelo MEA e pelo método ASTM D 54353:2012 (certificado). As concentrações são expressas com média ± desvio padrão (n = 3)……………………... 68 Tabela 10. Determinação de enxofre como CS em 258,056 nm (PC ± 1) em amostras de diesel por MEA. Incertezas são expressas com intervalo de confiança de 95 % (n = 3). A recuperação de enxofre é expressa como porcentagem de recuperação de massa de enxofre adicionada na amostra (tioureia) com posterior determinação…………….. 69  e C 2  -por HR CS GFMAS, em diferentes transições vibracionais (v', v''). O deslocamento isotópico foi calculado pela Equação 3 e convertido em comprimento de onda para avaliar sua correlação com os dados experimentais. O valor de deslocamento isotópico entre parêntesis no comprimento de onda 600,24 nm corresponde ao observado experimentalmente………………...…. 110 Tabela 19. Determinação de bromo por SS-HR CS GFMAS por calibração externa e por ID. As incertezas experimentais são expressas como intervalo de confiança de 95 % (n = 5)……………………………………………………………………………….. TIMS -MS com ionização térmica (thermal ionization MS)TXRF -Fluorescência de raios-X por reflexão total (total reflexion X-ray fluorescence)

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Spectrometric methods for the determination of chlorine in crude oil and petroleum derivatives — A review

Cited by 27 publications

References 29 publications

Determination of Chlorine in Crude Oil Emulsified via the MgCl Molecule by HR‑CS MAS

Determination of Chlorine in Crude Oil Emulsified via the MgCl Molecule by HR‑CS MAS

Evaluation and determination of chloride in crude oil based on the counterions Na, Ca, Mg, Sr and Fe, quantified via ICP-OES in the crude oil aqueous extract

Desenvolvimento de procedimentos analíticos para a determinação de não-metais via moléculas diatômicas por espectrometria de absorção molecular de alta resolução com fonte contínua

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