A New Sensor Based on Reduced Graphene Oxide/Au Nanoparticles for Glycerol Detection

Assis, Kelly Leite dos Santos Castro; Archanjo, Braulio S.; Achete, Carlos Alberto; D’Elia, Eliane

doi:10.1590/1980-5373-MR-2019-0513

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Article • Mat. Res. 23 (2) • 2020 • https://doi.org/10.1590/1980-5373-MR-2019-0513 copy

A New Sensor Based on Reduced Graphene Oxide/Au Nanoparticles for Glycerol Detection

Authorship SCIMAGO INSTITUTIONS RANKINGS

Abstract

The projections for the global energy demand have been one of our society’s greatest challenges, which has contributed significantly to the search for new sources of energy, among which biodiesel stands out and, consequently, the development of methods for quality assurance is essential to ensure its technological demand. In this context, a stable sensor based on graphene oxide and gold nanoparticles was developed for glycerol analysis. The electrochemically deposited gold nanoparticles presented the best results with a peak current (I_p) four times greater than the chemically produced gold nanoparticles. The combination of glassy carbon electrode with electrochemically reduced graphene and electrochemically deposited gold nanoparticles (GCE-ErGO-EAuNp) resulted in an efficient sensor to detect glycerol, promoting an I_p increase. The proposed non-enzymatic method showed a linear response in the concentration range of 1.0 x 10^-3 to 1.0 x 10^-2%(w/w) with a good determination coefficient (r² = 0.9989), limits of detection and quantification at 1.2 x 10^-4% and 4.0 x 10^-4%(w/w), respectively, with a repeatability of (RSD% ranged from 0.36% to 2.78%), intermediate precision and recovery of (99.3% to 104.4%) and excellent stability of 700 continuous analysis cycles.

Keywords:
Biodiesel; Liquid-liquid Extraction; Graphene Oxide; Gold Nanoparticles; Glycerol; Cyclic Voltammetry; Validation

Theoretical [Glycerol] (% w/w)	1^st Signal	2^nd Signal	3^rd Signal	Average	Standard deviation	Standard deviation	Measured [Glycerol] (% w/w)	Error (%)
Theoretical [Glycerol] (% w/w)	(μC)	(μC)	(μC)	(μC)	(μC)	(μC)	Measured [Glycerol] (% w/w)	Error (%)
1.0 x 10^-3	7.76 x 10^-6	7.71 x 10^-6	7.75 x 10^-6	7.74 x 10^-6	2.81 x 10^-8	0.36	1.01 x 10^-3	100.6
2.0 x 10^-3	1.51 x 10^-5	1.51 x 10^-5	1.48 x 10^-5	1.50 x 10^-5	2.10 x 10^-7	1.40	2.09 x 10^-3	104.4
3.0 x 10^-3	2.17 x 10^-5	2.22 x 10^-5	2.10 x 10^-5	2.17 x 10^-5	6.03 x 10^-7	2.78	3.08 x 10^-3	102.8
4.0 x 10^-3	2.73 x 10^-5	2.76 x 10^-5	2.79 x 10^-5	2.76 x 10^-5	3.05 x 10^-7	1.11	3.97 x 10^-3	99.3
5.0 x 10^-3	3.45 x 10^-5	3.44 x 10^-5	3.45 x 10^-5	3.45 x 10^-5	4.00 x 10^-7	0.12	5.00 x 10^-3	99.9
6.0 x 10^-3	4.27 x 10^-5	4.26 x 10^-5	4.21 x 10^-5	4.25 x 10^-5	3.01 x 10^-7	0.71	6.19 x 10^-3	103.2
7.0 x 10^-3	4.94 x 10^-5	4.91 x 10^-5	4.86 x 10^-5	4.91 x 10^-5	3.91 x 10^-7	0.80	7.17 x 10^-3	102.7
8.0 x 10^-3	5.60 x 10^-5	5.62 x 10^-5	5.57 x 10^-5	5.60 x 10^-5	2.69 x 10^-7	0.48	8.21 x 10^-3	102.6
9.0 x 10^-03	6.16 x 10^-5	6.17 x 10^-5	6.09 x 10^-5	6.14 x 10^-5	4.61 x 10^-7	0.75	9.01 x 10^-3	100.2
1.0 x 10^-3	6.76 x 10^-5	6.82 x 10^-5	6.81 x 10^-5	6.79 x 10^-5	3.24 x 10^-7	0.48	9.99 x 10^-3	99.9

Reference	Sensor	Electrochemical technique	LOD	Linear range (mmol L^-1)
Reference	Sensor	Electrochemical technique	(mmol L¹1 Adzic RR, Hsiao MW, Yeager EB. Electrochemical oxidation of glucose on single crystal gold surfaces. J Electroanal Chem Interfacial Electrochem. 1989;260(2):475-85. http://dx.doi.org/10.1016/0022-0728(89)87164-5. http://dx.doi.org/10.1016/0022-0728(89)8... )	Linear range (mmol L^-1)
Maruta and Paixão¹⁶16 Maruta AH, Paixão TRLC. Flow injection analysis of free glycerol in biodiesel using a copper electrode as an amperometric detector. Fuel. 2012;91(1):187-91. http://dx.doi.org/10.1016/j.fuel.2011.06.071. http://dx.doi.org/10.1016/j.fuel.2011.06...	Au	FIA	0.0005	0.001 to 0.3
Li et al.¹⁸18 Li N, Zhou Q, Li X, Chu W, Adkins J, Zheng J. Electrochemical detection of free glycerol in biodiesel using electrodes with single gold particles in highly ordered SiO2 cavities. Sens Actuators B Chem. 2014;196(Suppl. C):314-20. http://dx.doi.org/10.1016/j.snb.2014.02.017. http://dx.doi.org/10.1016/j.snb.2014.02....	Si/Au	VPD-CA	0.0015	0.01 to 0.8
Yasmin et al.³¹31 Yasmin A, Luo J-J, Daniel IM. Processing of expanded graphite reinforced polymer nanocomposites. Compos Sci Technol. 2006;66(9):1182-9. http://dx.doi.org/10.1016/j.compscitech.2005.10.014. http://dx.doi.org/10.1016/j.compscitech....	C/NiNp	VPD-CA	0.033	0.5 to 12
Li et al.¹⁸18 Li N, Zhou Q, Li X, Chu W, Adkins J, Zheng J. Electrochemical detection of free glycerol in biodiesel using electrodes with single gold particles in highly ordered SiO2 cavities. Sens Actuators B Chem. 2014;196(Suppl. C):314-20. http://dx.doi.org/10.1016/j.snb.2014.02.017. http://dx.doi.org/10.1016/j.snb.2014.02....	Cu	FIA-CA	0.003	0.033 to 1.7
Chen et al.⁴⁸48 Chen W-C, Li P-Y, Chou C-H, Chang J-L, Zen J-M. A nonenzymatic approachfor selective and sensitive determination of glycerol in biodiesel based on a PtRu-modified screen-printed edge band ultramicroelectrode. Electrochim Acta. 2015;153:295-9. http://dx.doi.org/10.1016/j.electacta.2014.12.011. http://dx.doi.org/10.1016/j.electacta.20...	PtRu-SPUME	CA	0.006	0.01 to 1
This Work	ErGO/EAuNp	CV	0.01	0.1 to 1.1

Biodiesel	GC	Electrochemical method	Recovery
Sample	(%w/w)	(%w/w)	(%)
1	0.0060 ± 0.0005	0.0060 ± 0.0002	99.84
2	0.0180 ± 0.0005	0.0174 ± 0.0005	96.82
3	0.0019 ± 0.0005	0.0018 ± 0.0001	96.82

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