Smart Electrochemical Portable Tools for Cultural Heritage Analysis: A Review
Abstract
:1. Introduction
2. Electrochemical Impedance Spectroscopy in CH
EIS for Evaluating Corrosion Events and Analyzing Metallic Protective Layers of CH Objects and Surfaces
3. Electrochemical Devices to Apply in CH
3.1. Electrochemical Small Tools to Apply in Diagnosis and Preservation of CH
Portable Electrochemical Sensor Prototypes in CH Field Applications
3.2. Portable Electrochemical Immunosensors to Apply in CH Fields
3.3. Portable Electrochemical Biosensors to Apply in CH
4. Conclusions
Funding
Acknowledgments
Conflicts of Interest
References
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Original Metal Samples | Equivalent Circuit (ECs) and Electrical Elements | Real Case of Study: Original Metal Coatings/Layers | References |
---|---|---|---|
Clean metals | Randles circuit with Re that is the electrolyte resistance; CPEdl is the double-layer capacitance; Rct is the charge transfer resistance, and finally W is the Warburg impedance for copper ions, during their diffusion through the oxide film | The Randles circuit was analytically standardize and validated, by using the standard corrosion events of copper in slightly mineralized neutral aqueous solutions (such as tap water, as conventional working medium) | [60,61] |
Clean metals | A variation of the previous Randles circuit consists of the charge transfer resistances of cathodic and anodic processes, are in parallel in different branches of the circuit | The EIS spectra, acquired with the modified Randles circuit, was applied to recorded EIS profiles for artistic bronze coupons in artificial rain | [60] |
Clean metals | Other authors have applied a simple two nested (R-CPE) couple circuit, but fitting results showing the exponent of the second CPE close to 0.5, suggesting a diffusion impedance, both in copper and brass | Copper and brass surfaces for application of the two nested (R-CPE) couple of electrochemical circuits | [62,63,64] |
Metals with patinaCopper and alloys | The first EC (where the pair CPEdl-Rct is not considered to be electrical equivalent element) represents the double-layer patina morphology, quite similar to the anodized layers in aluminum model, which consist of a thin barrier layer covered by a porous outer layer | This equivalent circuit describes the outdoor copper and bronze patinas, exhibiting a double-layer structure. In particular, the inner layer contains cuprous oxide materials and an outer layer, appears more porous for the presence of different cupric compounds, depending on the environment to which the object is exposed and located | [65] |
Metals with patina Copper and alloys | The second EC with two nested (R-CPE) couple circuit, represents the impedance of the inner and outer patina layer. Considering an exponent value of 0.5 for the CPE in the inner layer, a Warburg/W impedance, could replace the CPE final circuit. | The same EC was applied to study the response of bronze roman coins and natural copper patinas, formed during 1–3 years in Chile in different environments, with different thickness and porosity depending on their location | [66] |
Metals with patina Copper and alloys | Three nested (R-CPE) circuits were reported in the literature, to explain the electrochemical output signals regarding artificial patinas, putting in Na2SO4-NaHCO3, as working electrolytes. The first (R-CPE) pair represents the resistance and capacitance of the patina, the second (R-CPE), at intermediate frequencies, represents the corrosion process on the metal surface, while third (R-CPE) couple that corresponds to the low-frequency loop is explained as a result of oxidation–reduction processes of the corrosion products taking place at the electrode surface | A first example of this three nested (R-CPE) circuits is the EIS spectrum profiles of samples, collected by a brass object, excavated from the archaeological area of Tharros, in 0.1 M NaCl (as working electrolyte). Another example concerns archaeological bronze coins, working with NaCl 0.3 M-5% agar electrolyte and mineral water. This EC is depicted in a different order (Re[(Rct-CPEdl)(Rpl-CPEpl)]) that is mathematically. Equivalent as EC and which best represents the original sample | [67,68,69,70,71] |
Metals with patina Iron and steel | Two-cell EC have been applied to describe the impedance of the two interfaces: metal/rust layer and rust layer/electrolyte, respectively. A third time constant seems to be present at low frequencies, applying the R(RC(C[RW])) model and performing measurements in the G-PE cell | Regarding the Two-cell EC circuits electrochemical studies were carried out on weathering steel sculptures from Adriana Veyrat; Politecnico di Torino performed EIS measurements on historic iron surface/coating belonging to the Notre-Dame Cathedral of Amiens and the Metz Cathedral, in France | [72] |
Evaluation of coatings | A metal-coating system is a capacitor and a resistance in parallel, according to the capacitance (Ccoat) and resistance (Rcoat) of the metal coating in series with the resistance of the working electrolyte, (Re). In highly protective coatings, Rcoat is very high and the system becomes Ccoat in series with Re (no current crosses the resistance). When the coating deteriorates the circuit, changes and the main electric components/elements are Cdl (the double-layer capacitance and Rct (the charge transfer resistance) of the corrosion process that occurs at the metal-electrolyte interface. This circuit was applied to the characterization of organic coatings, including varnishes and waxes for bronze and historic steel artwork objects | Not reported cases of studies on original samples | [73,74,75] |
Evaluation of inhibitors | The EC circuits are the same of the clean surfaces, only differing in the values of different parameters | Not reported cases of studies on original samples | [76,77] |
Electrochemical Configurations | Quantitative Analysis | Qualitative Analysis | Main Advantages | Main Disadvantages |
---|---|---|---|---|
Setup1: | ---------------------------- | ✓ | easy sensor geometry for in situ manipulation | Stiff (not flexible) contact probe and the liquid conductive electrolytes provoke electrochemical contact problems toward the surface of cultural heritage, compromising the final electrochemical measurements |
Setup2: | ---------------------------- | ✓ | Flexible cell geometries suitable for CH surfaces (with significant roughness) Solid conductive electrolytes to guarantee the electrochemical/electrical contact toward CH surfaces | The difficulty of processing the acquired experimental data by ECs, working with Nyquist plot |
Sample As(III) | GO/SPEs by SWCSV (μg/L) | Total Inorganic As: [As(III) + As(V)] Total Inorganic Fe: [FeO + Fe3O4 + Fe2O3] (μg/L) | ICP-MS (μg/L) | P Value (t-Test)a |
---|---|---|---|---|
1 | 992 ± 2 | 101 ± 2 | 100.80 ± 0.5 | 0.01 |
2 | 100 ± 1 | 100 ± 1 | 100.00 ± 0.02 | 0.03 |
3 | 102 ± 2 | 103 ± 1 | 103.05 ± 0.5 | 0.02 |
Sample Fe(III) | ||||
1 | 399 ± 1 | 400 ± 1 | 400 ± 1 | 0.04 |
2 | 400 ± 2 | 400 ± 2 | 400 ± 0,2 | 0.01 |
3 | 402 ± 1 | 403 ± 0.3 | 403 ± 1 | 0.03 |
Electrochemical Devices | Quantitative Analysis | Qualitative Analysis | Main Advantages | Main Disadvantages |
---|---|---|---|---|
Raman spectrometer, equipped with a potentiostatic apparatus | LOD = 5 ppm (mg/L) for melamine | ✓ | low cost measurement, no-time consuming analysis, high sensitivity, low detection of limit | Non-electroactive pigments and organic binders cannot quantify by electrochemistry |
Electrochemical cell, which also works like a Bragg tool | ---------------------------- | ✓ | to detect different crystallographic phases during serious corrosion events, to detect the corrosion potential Ecorr, both parameters, unequivocally provide important information on the nature of metallic corrosion phenomena | not all the corrosion products, to which different crystallographic phases belong, have electrochemical activity, therefore the disadvantage is that there is only qualitative crystallographic information |
Screen-Printed Electrodes (SPEs) chemically modified with Graphene Oxide (GO); GO/SPE | See Table 3 | ✓ | Voltammetric techniques are useful to understand two important aspects, as -the chemical-physical composition of the colors; -the oxidation status and conservation conditions of metallic elements contained in organic pigments, useful to select the best restoration strategies | Particularly useful only in the case of metals contained in inks, colored pigments and organic compounds The absence of metals makes the application of this device more difficult, as the organic component (very often) does not have a marked electrocatalytic activity |
micro-sample coatings in Paraloid B72 film-modified electrodes, combined with | ---------------------------- | ✓ | micro-sample coatings in Paraloid B72-film provide the possibility of pre-concentrating the pigments to increase the Signal/Noise ratio, especially in the presence of traces of organic materials | micro-sample coatings in Paraloid B72-film are not so selective and for this purpose several interferences and/or passivation/fouling effects can occur during analysis/measurements |
Immunosensor Prototype | Quantitative Analysis | Qualitative Analysis | Main Advantages | Main Disadvantages |
---|---|---|---|---|
Nano-Electrode Ensembles (NEEs) immunosensors for the detection of ovalbumin in paintings | ✓ | ----------------------------------- | High selectivity and specificity for the proteins and organic binder recognition, more than FTIR traditional method | No quantification of the organic component in paintings and this could represent a lack of useful information for restorers |
Nano-Electrode Ensembles (NEEs) immunosensors for the detection of egg yolk in tempera and paintings | ✓ | ----------------------------------- | High selectivity and specificity for the proteins and egg yolk recognition, more than FTIR traditional method | No quantification of the organic component in paintings and this could represent a lack of useful information for restorers |
Scanning Electro-Chemical Microscopy (SECM) immunosensors | ✓ | ------------------------------------ | Immunochemical stratigraphic SECM is excellent to selectively identify the organic components in the painting layers | Low reproducibility due to the passivation/fouling of the scanning/electrode-based tip Low Signal/to Noise Ratio |
Biosensor Prototype | Quantitative Analysis | Qualitative Analysis | Main Advantages | Main Disadvantages |
---|---|---|---|---|
Impedance biosensor devices, recording Faradaic signal, in the presence of the electroactive probes | ✓ | Linear range of concentration: 6.0 × 104–6.0 × 107 cells/mL; Limit Of Detection (L. O. D.): 6.0 × 102 cells/mL. | High selectivity and sensitivity toward the organic binder recognition, more than FTIR traditional method. The biosensor regeneration opportunity | The inadequacy, in some case studies, of the Randles model equivalent electrical circuit to describe the electrochemical impedance biosensor prototypes |
Impedance biosensor devices, recording non-Faradaic signal, without the electroactive probes | ✓ | Linear range of concentration: 104–107 cfu/mL; Limit Of Detection (L. O. D.): 1.0 × 102 cells/mL. | High Signal/Noise ratio Lower LOD | Possible Fouling and passivation phenomenon with interference on the output signals due to the stable chemical bonds between bacteria suspension and the immobilized antibodies |
Surface Plasmon Resonance-based biosensors | ✓ | The direct assay of albumen/yolk mixture recognized the presence of both chemical analytes (140.0 ± 5.6 RU) for (anti-OVA) channel, (123.3 ± 4.9 RU) for (anti-IgY) channel. | The experimental results confirmed that very short application times were enough to extract useful information and, at the same time, they were ideal for avoiding invasive treatments on original artwork surfaces | The main analytical problem could be related to the interference when in absence of Highly Viscous Polymeric Dispersions (HVPDs) extracts from original samples |
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Valentini, F. Smart Electrochemical Portable Tools for Cultural Heritage Analysis: A Review. Sensors 2019, 19, 4303. https://doi.org/10.3390/s19194303
Valentini F. Smart Electrochemical Portable Tools for Cultural Heritage Analysis: A Review. Sensors. 2019; 19(19):4303. https://doi.org/10.3390/s19194303
Chicago/Turabian StyleValentini, Federica. 2019. "Smart Electrochemical Portable Tools for Cultural Heritage Analysis: A Review" Sensors 19, no. 19: 4303. https://doi.org/10.3390/s19194303