Abstract

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 (Ip) 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 Ip 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.

Highlights

  • IntroductionGlycerol is a water-soluble product that is viscous, hygroscopic, odourless and has a sweet taste; it is a natural chemical constituent of many foods and is currently used in fruit juices, wine, vegetable oil, beer, tobacco, honey, among others[1,2,3,4]

  • Glycerol is a water-soluble product that is viscous, hygroscopic, odourless and has a sweet taste; it is a natural chemical constituent of many foods and is currently used in fruit juices, wine, vegetable oil, beer, tobacco, honey, among others[1,2,3,4].The determination of glycerol has been used in many applications, such as clinical, pharmaceutical and food-industry laboratories, and more recently in biodiesel quality control

  • The official methods for determining glycerol are those recommended by the Association of Official Analytical Chemists (AOAC) involving gas and liquid chromatography, which are time-consuming, tedious and expensive to use for routine analysis[3]

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Summary

Introduction

Glycerol is a water-soluble product that is viscous, hygroscopic, odourless and has a sweet taste; it is a natural chemical constituent of many foods and is currently used in fruit juices, wine, vegetable oil, beer, tobacco, honey, among others[1,2,3,4]. The development of accessible devices is necessary for the field’s research advancement, which enables the development of alternative commercial techniques for the determination of this analyte In this context, the enzymatic methods that combine the selectivity of enzymes involved are either ‘in solution’ or ‘immobilized’, and different detection systems have been extensively applied to develop prospective methods for measuring glycerol in clinical analysis, food products and biotechnological processes[4,5,6,7,8,9,10,11,12,13]. Materials Research called catalyst poisoning and one of the main problems of the use of metals in organic molecules electroanalysis, generating the loss of electric signals as a result, which decreases the sensitivity of the electrode In this context, the gold is an excellent catalyst for the electro‐oxidation of organic molecules, like glycerol, because it promotes good stability and sensitivity. Sensors based on reduced graphene oxide (rGO) and gold nanoparticles (AuNp) were studied to detect free glycerol in biodiesel previously extracted by liquid phase extraction

Graphene Oxide Sample Preparation
Characterization of expanded graphite and graphite oxide
Gold nanoparticles preparation
Characterization of GCE modified electrodes
Partial validation of proposed method
Linearity
Limit of detection and Limit of quantification
2.12 Biodiesel analysis
Sensors characterization and Glycerol electro-oxidation
Real sample analysis with the sensor proposed in this work
5.Conclusions
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