Determination of nutrients and potentially toxic elements in Jatropha curcas seeds, oil and biodiesel using inductively coupled plasma mass spectrometry

Maciel, P. B.; Barros, Lucicléia; Duarte, Estela; Harder, Márcia Nalesso Costa; Bortoleto, Gisele Gonçalves; Abreu-Junior, Cassio Hamilton; Villanueva, Felipe Carlos Alvarez

doi:10.1007/s10967-012-2365-y

Cited by 11 publications

(4 citation statements)

References 6 publications

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“…Three samples of crude glycerol from biodiesel production were analyzed, two samples were obtained from the biodiesel industry, and another by the transesterification of Jatropha curcas oil (Maciel et al, 2013).…”

Section: Crude Glycerol Samplesmentioning

confidence: 99%

Determination of methanol residues in crude glycerol for animal feed by gas chromatography

Nazato

Romero

Abdalla

2019

Sci. agric. (Piracicaba, Braz.)

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Crude glycerol is a major by-product of biodiesel production and is an economical additive feed for ruminants. However, residual methanol in crude glycerol can be harmful to animal health. Several methods exist for quantifying methanol residues in biodiesel, yet few have been described that identify the methanol level in crude glycerol. We propose a method for determining the methanol level in crude glycerol destined for animal feed. Crude glycerol was extracted from the headspace and quantified by gas chromatography using a flame ionization detector (GC-FID). The method was linear up to 0.5 % of methanol. The limits of detection (LOD) and quantification (LOQ) were 0.015 and 0.031 %, respectively. No significant matrix effects were observed. Precision was 2 % at the 0.05 and 0.5 % levels. The average percentage of recovery was 90 %. Three analyzed samples of crude glycerol had methanol residues of 0.027-7.802 %. Furthermore, this methanol quantification method may be externally or internally calibrated using a GC manual injector. A reduction of at least 20 % in running time was obtained with good resolution between the peaks. Thus, this method can be applied to determine the methanol level in crude glycerol according to the upper limits for animal feed (5,000 ppm) and for human consumption (150 ppm). Finally, this method is useful for the quality control of crude glycerol intended for use in animal feed, enabling the alternative use of this by-product to add value to the biodiesel production chain.

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Section: Crude Glycerol Samplesmentioning

confidence: 99%

Determination of methanol residues in crude glycerol for animal feed by gas chromatography

Nazato

Romero

Abdalla

2019

Sci. agric. (Piracicaba, Braz.)

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“…Total decomposition of samples [4][5][6][7][8] and their introduction in the equipment in the form of emulsions or microemulsions [9][10][11][12] are very popular, despite some problems verified in their application. Extraction methods are also available for the determination of trace elements in organic liquids [13][14][15][16].…”

Section: Introductionmentioning

confidence: 99%

Development of a method for total Hg determination in oil samples by cold vapor atomic absorption spectrometry after its extraction induced by emulsion breaking

Vicentino

Brum

Cassella

2015

Talanta

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This work reports the development of a novel extraction method for total Hg determination in oil samples. After extracting Hg from samples it was quantified in the extracts by cold vapor atomic absorption spectrometry (CV-AAS), employing a laboratory-made gas-liquid separator (GLS) and NaBH4 as reducing agent. The extraction of Hg from samples was carried out by extraction induced by emulsion breaking (EIEB), which is based on the formation and breaking of water-in-oil emulsion between the oil samples and an extractant solution containing an emulsifying agent (surfactant) and nitric acid. Operational parameters of the GLS were evaluated in order to set the best performance of the measurement system. In these studies it was proven that the volume of sample and the concentration of HCl added to the sample extracts had significant influence on Hg response. The best conditions were achieved by adding 0.5 mL of a 0.3 mol L(-1) HCl solution on 1 mL of sample extract. The extraction conditions were also optimized. The highest efficiency was observed when 4 mL of a solution containing 2.5% triton X-100 and 15% v/v HNO3 were employed for the extraction of Hg contained in 20 mL of sample. Emulsion breaking was performed by heating at 80 °C and took approximately 20 min. The limit of quantification of the method was 1.9 µg L(-1) and recovery percentages between 80% and 103% were observed when spiked samples (2 and 10 µg L(-1)) of diesel oil, biodiesel and mineral oil were analyzed.

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“…Dilution in an organic solvent (i.e., ethanol, xylene, or kerosene) has been widely recommended for the determination of Na, Ca, K, and Mg by AAS or ICP-OES. − Unlike FAAS, the latter technique has multielemental capability, and it provides lower limits of detection and wider dynamic ranges than the former. However, the introduction of organic samples into the plasma is a challenging subject, as ICP techniques suffer from severe interference caused by complex organic matrices (e.g., matrix effects, plasma degradation, or soot deposition at the injector tip). − To circumvent this, several sample preparation approaches have been developed, such as acid digestion and sample oxidation or combustion. ,, However, these methods show some problems caused by addition of reagents, sample contamination, degradation of limits of detection (LODs), and volatile compound losses.…”

mentioning

confidence: 99%

Aerosol-Phase Extraction Method for Determination of Ca, K, Mg, and Na in Biodiesel through Inductively Coupled Plasma Optical Emission Spectrometry

et al. 2017

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A novel extraction method was developed, optimized, and validated for the elemental analysis of organic samples. The method, called aerosol-phase extraction (APE), is based on nebulization of the extracting aqueous solution (0.1 mol·L nitric acid) on the sample. Extraction was performed at the interface of generated extractant droplets as they entered into contact with the samples. Afterward, the phases were allowed to separate and Ca, K, Na, and Mg were determined in aqueous phase by means of inductively coupled plasma optical emission spectroscopy (ICP-OES). Measurement of aerosol characteristics demonstrated that a water-in-oil emulsion was generated. Therefore, once the aqueous solution was dispersed into the sample, the phases spontaneously separated. Furthermore, the interfacial specific surface area exhibited values on the order of 1 m·mL, hence enhancing the extraction kinetics over conventional extraction methods. Key variables affecting the extraction yield were the nebulization gas flow rate, liquid flow rate, extraction time, acid concentration, nebulizer tip to sample surface gap, and m/m ratio. Once the optimal conditions were selected, the method was applied and validated for the determination of Ca, K, Na, and Mg by ICP-OES in 0.5 mL biodiesel samples with an expanded uncertainty lower than 2%. With the APE method, the extraction time was around 1 min, whereas conventional methods employed to perform this kind of extraction required from 4 to 50 min. Additionally, the APE involved preconcentration of analytes, thus lowering the limit of detection (LOD) to the nanograms per milliliter level (i.e., LODs based on the 3s criterion were 32, 20, 19, and 24 ng·mL for Ca, K, Na, and Mg, respectively). Furthermore, accuracy of quantification of Ca, K, Na, and Mg concentration by APE was not significantly different as compared to that afforded by conventional liquid-liquid extraction. Finally, Ca, K, Na, and Mg contents were determined in four real samples in the 0.5-13 mg·kg range. The obtained results were not statistically different from those encountered with a microwave-based digestion method.

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Determination of nutrients and potentially toxic elements in Jatropha curcas seeds, oil and biodiesel using inductively coupled plasma mass spectrometry

Cited by 11 publications

References 6 publications

Determination of methanol residues in crude glycerol for animal feed by gas chromatography

Determination of methanol residues in crude glycerol for animal feed by gas chromatography

Development of a method for total Hg determination in oil samples by cold vapor atomic absorption spectrometry after its extraction induced by emulsion breaking

Aerosol-Phase Extraction Method for Determination of Ca, K, Mg, and Na in Biodiesel through Inductively Coupled Plasma Optical Emission Spectrometry

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