Determination of Ca, Mg, Sr and Ba in crude oil samples by atomic absorption spectrometry

Pessoa, Helen Moura; Hauser‐Davis, Rachel Ann; Campos, Reinaldo Calixto de; Castro, Eustáquio Vinícius Ribeiro de; Carneiro, Maria Tereza Weitzel Dias; Brandão, Geisamanda Pedrini

doi:10.1039/c2ja30125c

Cited by 17 publications

(9 citation statements)

References 23 publications

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“…A simple emulsion protocol for the determination of Ba, Ca, Mg and Sr in crude oils using FAAS (for Ca, Mg and Sr) and ETAAS (for Ba) was described by Pessoa et al 79 The amount of sample required was dependent on the analyte, but was approximately 0.1 g, 0.25 g and 1 g for Mg, Ca and Sr respectively. Sample was diluted with 1 mL of toluene, sonicated using a sonic bath for ve min and then Triton X-100 (100 mg) and potassium chloride (0.5 mL of 2%) added.…”

Section: Fuels and Lubricantsmentioning

confidence: 99%

Atomic spectrometry update: review of advances in the analysis of metals, chemicals and materials

Carter

Clough

Fisher

et al. 2018

J. Anal. At. Spectrom.

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Section: Fuels and Lubricantsmentioning

confidence: 99%

Atomic spectrometry update: review of advances in the analysis of metals, chemicals and materials

Carter

Clough

Fisher

et al. 2018

J. Anal. At. Spectrom.

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“…The metals and non-metals contained in crude oil can cause corrosion and encrustation in distillation towers as well as poisoning of catalysts and environmental pollution [6][7][8]. Special attention is paid to corrosion caused by the presence of inorganic contaminants (chloride salts) in crude oil.…”

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%

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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“…Digestion procedures to eliminate the organic matrix of crude oil samples are frequently performed to obtain a suitable aqueous solution for the analysis by inductively coupled plasma optical emission spectrometry (ICP OES) but this procedure is prone to contamination or analyte loss [8,9]. Alternative procedures for crude oil sample preparation have been proposed to reduce cost and time analysis, simplifying this step [10].…”

Section: Introductionmentioning

confidence: 99%

Extraction induced by emulsion breaking for determination of Ba, Ca, Mg and Na in crude oil by inductively coupled plasma optical emission spectrometry

Trevelin

Marotto

Castro

et al. 2016

Microchemical Journal

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a b s t r a c tThe selection of the sample preparation method is one of the most critical steps in the determination of metals using atomic spectrometry techniques. The aim of this paper was to propose the use of a novel strategy for crude oil sample preparation, based on the extraction induced by emulsion breaking, prior to the determination of Ba, Ca, Mg and Na by inductively coupled plasma optical emission spectrometry (ICP OES). The emulsions were prepared by mixing the crude oils samples diluted in xylene with 5% m/v Triton X-100 solution in 10% v/v HNO 3 . The emulsion breaking was performed by heating at 80 ± 2°C following by centrifugation to improve the separation, resulting in two distinct phases. The aqueous phase was analysed by ICP OES using inorganic standards solutions for external calibration. Ba, Ca, Mg and Na were totally extracted at a single extraction step. The limits of detection were 0.12, 1.2, 0.14 and 5.8 μg L −1 for Ba, Ca, Mg and Na, respectively. The percentage recoveries ranged from 99 to 104% and the good agreement with the values of the certified reference material (NIST 1634c), when student-t test was applied at 95% confidence limit (p b 0.05), warranted the accuracy of the procedure.

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Determination of Ca, Mg, Sr and Ba in crude oil samples by atomic absorption spectrometry

Cited by 17 publications

References 23 publications

Atomic spectrometry update: review of advances in the analysis of metals, chemicals and materials

Atomic spectrometry update: review of advances in the analysis of metals, chemicals and materials

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

Extraction induced by emulsion breaking for determination of Ba, Ca, Mg and Na in crude oil by inductively coupled plasma optical emission spectrometry

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