Simple Spectrophotometric Determination of Iron in Diesel Oil after Sample Preparation Employing Extraction Induced by Emulsion Breaking

Pereira, Thamiris V.; Cassella, Ricardo J.

doi:10.21577/0103-5053.20220046

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Article • J. Braz. Chem. Soc. 33 (10) • Oct 2022 • https://doi.org/10.21577/0103-5053.20220046 copy

Simple Spectrophotometric Determination of Iron in Diesel Oil after Sample Preparation Employing Extraction Induced by Emulsion Breaking

Authorship SCIMAGO INSTITUTIONS RANKINGS

This work reports the development of a simple and fast method for the spectrophotometric determination of Fe in diesel oil using the classic reaction with 1,10-phenanthroline after its extraction induced by emulsion breaking (EIEB). The extraction parameters of EIEB were optimized (concentration of HNO₃ and Triton X-100^® in the emulsifying solution) as well as the adjustment of the pH of the final solution, a necessary step to complete the colorimetric reaction. The developed method presented a limit of detection of 0.004 mg L^-1 and a limit of quantification of 0.013 mg L^-1 and was applied in the analysis of six samples of diesel oil with different specifications. The results were statistically similar to those obtained by graphite furnace atomic absorption spectrometry (GF AAS). A recovery test was also performed by spiking the samples with 1.0 mg L^-1 of Fe in the form of an organometallic compound, yielding recovery percentages between 83 and 108%.

Keywords:
diesel oil; spectrophotometry; iron; extraction induced by emulsion breaking

Sample preparation approach	Analytical technique	LOD/LOQ	Reference
Diesel oil mineralization using an optimized method based on focused microwave irradiation	ICP OES	0.14 µg g^-1/ LOQ not reported	¹²12 Sant’Ana, F. W.; Santelli, R. E.; Cassella, A. R.; Cassella, R. J.; J. Hazard. Mater. 2007, 149, 67.
Extraction induced by emulsion breaking followed of GF AAS determination	GF AAS	183 ng L^-1/ 609 ng L^-1	¹⁷17 Cassella, R. J.; Brum, D. M.; Paula, C. E. R.; Lima, C. F.; J. Anal. At. Spectrom. 2010, 25, 1704.
Direct injection of samples diluted with xylene	ICP OES	2.27 and 1.73 µg g^{-1 a}	³⁷37 Ulrich, A.; Wichser, A.; Anal. Bioanal. Chem. 2003, 377, 71.
Acid decomposition of samples in a closed-vessel microwave oven^b	ICP-MS	1.28 µg g^-1/ LOQ not reported	³⁸38 Bettinelli, M.; Spezia, S.; Baroni, U.; Bizzarri, G.; J. Anal. At. Spectrom. 1995, 10, 555.
Analyte extraction with diluted solutions of nitric acid using a counter current system	ICP-MS	0.1-3000 µg g^{-1 c}	³⁹39 Maryutina, T. A.; Soin, A. V.; Anal. Chem. 2009, 81, 5896.
Extraction of iron by EIEB followed of spectrophotometric determination with 1,10-phenanthroline	spectrophotometry	0.004 mg L^-1/ 0.013 mg L^-1	this work

Sample	Type	Fe concentration proposed method / (mg L^-1)	Fe concentration reference GF AAS method^a / (mg L^-1)
D₁	S10	0.092 ± 0.011	0.095 ± 0.008 (t = 0.408)
D₂	S10	0.30 ± 0.02	n.d.
D₃	S10	0.21 ± 0.02	0.20 ± 0.03 (t = 0.306)
D₄	S500	0.65 ± 0.04	0.60 ± 0.02 (t = 1.75)
D₅	S500	0.57 ± 0.03	n.d.
D₆	S500	0.42 ± 0.04	n.d.

Sample	Type	Recovery / %
D₁	S10	108 ± 8
D₂	S10	83 ± 11
D₃	S10	90 ± 7
D₄	S500	93 ± 5
D₅	S500	89 ± 8
D₆	S500	93 ± 6

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[1] *e-mail: rcassella@id.uff.br