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Nanostructured Co3O4 with near-cubic morphology was synthesised using the solvothermal method, and a non-enzymatic electrochemical glucose sensor (Co3O4–CuNPs/Pt) was successfully constructed by dropping and potentiostatic depositing technologies. The obtained Co3O4 and Co3O4–CuNPs were characterised and investigated by X-ray powder diffraction, scanning electron microscopy, transmission electron microscopy, energy dispersive X-ray spectroscopy and X-ray photoelectron spectroscopy. Quantitative analysis of glucose was performed using the amperometric (i–t) method, and a plot of current difference versus concentration of glucose was linear in the range 0.5–336 μM, with a linear correlation coefficient (R2) of 0.9989 and limit of detection (LOD) of 0.43 μM. When the linear range was reduced to 0.5–76.5 μM, R2 and LOD were 0.9997 and 0.17 μM, respectively. The sensitivity of the sensor was evaluated as 3.58 × 104 and 4.03 × 104 μA μM−1 cm−2 for the above two linear ranges, respectively. This novel sensor produced satisfactory reproducibility and stability and was applied to monitor trace amounts of glucose in human serum samples.

A novel modified electrode has been successfully constructed with the use of a nano-composite mixture consisting of molybdenum disulfide (MoS2) and gold nanoparticles (AuNPs). Its application as a cholesterol biosensor was investigated. The morphology of the prepared MoS2-AuNPs nanoparticles were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), atomic force microscope (AFM), X-ray diffraction (XRD) and energy dispersive X-ray spectroscopy (EDS). The physicochemical properties of the modified electrode at each stage of the construction were characterized by electrochemical impedance spectroscopy (EIS) and cyclic voltammetry (CV). Quantitative analysis of cholesterol was carried out with the use of the amperometric i–t method, and the calibration plot for cholesterol was linear in the range of 0.5–48 μM with a limit of detection (LOD) of 0.26 ± 0.015 μM. The apparent Michaelis-Menten constant ( K M a p p ) and sensitivity were estimated to be 0.325 mM and 4460 μA mM−1 cm−2, respectively. This novel sensor produced satisfactory reproducibility and stability, and was used successfully for the quantitative analysis of cholesterol in egg yolk and pork liver samples.

A novel 3D nano-flower-like Cu/multi-layer molybdenum disulfide composite (CuNFs/MoS2) modified glassy carbon electrode (GCE) has been successfully constructed. It was a highly sensitive and selective non-enzymatic hydrogen peroxide (H2O2) and glucose biosensor. The morphology of the obtained CuNFs-MoS2 nano-particles was investigated with the use of a scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD) and energy dispersive X-ray spectroscopy (EDS). The physicochemical properties of the modified electrode were characterized at each of the construction stages with the use of an electrochemical impedance spectroscopy (EIS) and cyclic voltammetry (CV) techniques. The new sensor combined the advantages of MoS2 and CuNFs, and exhibited high electro-catalytic activity toward H2O2 and glucose. Quantitative analysis of H2O2 and glucose was carried out with the use of the amperometric i-t method. Linear ranges were obtained between 0.04-1.88 μM and 1.88-35.6 μM for H2O2 and 1-20 μM and 20-70 μM for glucose, and their corresponding limits of detection (LOD) were 0.021 μM and 0.32 μM. This novel sensor was successfully applied for the quantitative analysis of H2O2 in tap water and glucose in human serum samples.

Bulk graphitic carbon nitride (g-C3N4) was obtained by pyrolysis of urea at 600 °C. The material was then subjected to protonation and exfoliation to obtain strongly fluorescent g-C3N4 nanosheets. These nanosheets are representing a two-dimensional layered material that emits strong blue fluorescence peaking at 434 nm, and their quantum yield of up to 10.3 % is much higher than that of bulk g-C3N4 (6.0 %). It was found that Cu(II) ions quench the fluorescence of the nanosheets due to photo-induced electron transfer (PET), probably the result of the stronger binding affinity between Cu(II) and the nitrogen and oxygen functional groups of the nanosheets. The probe responds to Cu(II) in the 0.01 to 0.4 nM concentration range, with a 8 pM detection limit. The method was applied to the determination of Cu(II) in spiked water samples.

A novel electrochemical sensor was constructed by depositing copper/copper oxide nano-particles on a glassy carbon electrode (GCE) to produce a Cu@CuO/GCE. The morphology and composition of this modified electrode were characterized with the use of scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDS), and X-ray diffraction (XRD) techniques. The electrochemical properties of the novel modified GCE electrode were studied using various electrochemical techniques such as cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS). The catalytic performance of the sensor was studied with the use of differential pulse voltammetry (DPV) under optimized conditions. The constructed Cu@CuO/GCE sensor showed significantly better electrocatalytic activity for the analysis of the H 2 O 2 in comparison to the Cu/GCE or GCE. The novel sensor produced a linear response for H 2 O 2 analysis in the range of 0.005–8 mM and the detection limit was 0.23 μM (S/N = 3). Satisfactory results were obtained for H 2 O 2 analyses of tap and lake waters. This performance compares very favorably with the results from several other commonly used techniques for analysis of H 2 O 2 .

A simple one-step electrodeposition method was used to construct a glassy carbon electrode (GCE), which has been modified with Cu doped gold nanoparticles (GNPs), i.e. a Cu@AuNPs/GCE. This electrode was characterized with the use of scanning electron microscopy (SEM) and X-ray diffraction (XRD) techniques. The eugenol was electrocatalytically oxidized at the Cu@AuNPs/GCE. At this electrode, in comparison with the behavior at the GCE alone, the corresponding oxidation peak current was enhanced and the shift of the oxidation potentials to lower values was observed. Electrochemical behavior of eugenol at the Cu@AuNPs/GCE was investigated with the use of the cyclic voltammetry (CV) technique, and additionally, in order to confirm the electrochemical reaction mechanism for o-methoxy phenols, CVs for catechol, guaiacol and vanillin were investigated consecutively. Based on this work, an electrochemical reaction mechanism for o-methoxy phenols was suggested, and in addition, the above Cu@AuNPs/GCE was successfully employed for the analysis of eugenol in food samples.

A novel Prussian blue/copper-gold bimetallic nanoparticles hybrid film modified electrode was prepared by electrochemical deposition on a glassy carbon electrode (PB/Cu-AuNPs/GCE). Morphology and electrochemistry of this electrode were studied by UV-vis spectroscopy, scanning electron microscopy, X-ray diffraction, cyclic voltammetry and electrochemical impedance spectroscopy. The sensor showed significantly better electrocatalytic activity for the reduction of hydrogen peroxide in comparison with the single PB/GCE and PB/AuNPs/GCE. This was attributed to the synergistic effect of PB and Cu-Au bimetallic nanoparticles. Also, the sensor demonstrated an overall high level of performance for the analysis of H2O2 in the concentration range from 0.002 to 0.84 mM.

Thermogravimetric analysis and differential scanning calorimetry have been applied to determine the adsorption of oil on selected adsorbates: sand, organo-clay and raw cotton. Thermal analysis provides evidence for the interaction and physical adsorption of the diesel oil on the adsorbates. Sand adsorbed diesel to around 33% by mass through weak physical interactions and appeared to fractionate the diesel components. The organo-clays more strongly adsorbed the diesel as evidenced by higher thermal decomposition temperatures. Differential scanning calorimetry (DSC) shows a strong interaction between the organo-clay and the diesel oil. Diesel is effectively adsorbed on organo-clay through adsorption and partitioning and is not removed from the organo-clay until significantly higher temperatures. Cotton displayed a very high adsorption/absorption capacity. A shift in the peak at 110°C (compared with pure diesel at 90°C) suggests an interaction between the diesel compounds and the cotton fibres as diesel is being retained at higher temperatures and more energy is required to evaporate the diesel. DSC was used to determine the strength of the diesel adsorption on the sand, organo-clay and cotton. The use of adsorbent materials to adsorb oil from oil spills is of great significance in modern society. One method of proving the effectiveness of an adsorbent material is through thermoanalytical techniques.

Studies of kaolinite surfaces are of industrial importance. One useful method for studying the changes in kaolinite surface properties is to apply chemometric analyses to the kaolinite surface infrared spectra. A comparison is made between the mechanochemical activation of Kiralyhegy kaolinites with significant amounts of natural quartz and the mechanochemical activation of Zettlitz kaolinite with added quartz. Diffuse reflectance infrared Fourier transform (DRIFT) spectra were analyzed using principal component analysis (PCA) and multi-criteria decision making (MCDM) methods, the preference ranking organization method for enrichment evaluations (PROMETHEE) and geometrical analysis for interactive assistance (GAIA). The clear discrimination of the Kiralyhegy spectral objects on the two PC scores plots (400–800 and 800–2030 cm−1) indicated the dominance of quartz. Importantly, no ordering of any spectral objects appeared to be related to grinding time in the PC plots of these spectral regions. Thus, neither the kaolinite nor the quartz are systematically responsive to grinding time according to the spectral criteria investigated. The third spectral region (2600–3800 cm−1, OH vibrations), showed apparent systematic ordering of the Kiralyhegy and, to a lesser extent, Zettlitz spectral objects with grinding time. This was attributed to the effect of the natural quartz on the delamination of kaolinite and the accompanying phenomena (i.e., formation of kaolinite spheres and water). The mechanochemical activation of kaolinite and quartz, through dry grinding, results in changes to the surface structure. Different grinding times were adopted to study the rate of destruction of the kaolinite and quartz structures. This relationship (i.e., grinding time) was classified using PROMETHEE and GAIA methodology.

This paper reviews the synthesis and the absorbing properties of the wide variety of porous sorbent materials that have been studied for application in the removal of organics, particularly in the area of oil spill cleanup. The discussion is especially focused on hydrophobic silica aerogels, zeolites, organoclays and natural sorbents many of which have been demonstrated to exhibit (or show potential to exhibit) excellent oil absorption properties. The areas for further development of some of these materials are identified.

The self-assembly of layered molybdenum disulfide-graphene (MoS2-Gr) and horseradish peroxidase (HRP) by electrostatic attraction into a novel hybrid nanomaterial (HRP-MoS2-Gr) is reported. The properties of the MoS2-Gr were characterized by X-ray diffraction (XRD), high-resolution transmission electron microscopy (TEM), electrochemical impedance spectroscopy (EIS) and cyclic voltammetry (CV). UV-vis and Fourier transform infrared spectroscopy (FT-IR) indicate that the native structure of the HRP is maintained after the assembly, implying good biocompatibility of MoS2-Gr nanocomposite. Furthermore, the HRP-MoS2-Gr composite is utilized as a biosensor, which displays electrocatalytic activity to hydrogen peroxide (H2O2) with high sensitivity (679.7 μA mM(-1)cm(-2)), wide linear range (0.2 μM-1.103 mM), low detection limit (0.049 μM), and fast amperometric response. In addition, the biosensor also exhibits strong anti-interference ability, satisfactory stability and reproducibility. These desirable electrochemical properties are attributed to the good biocompatibility and electron transport efficiency of the MoS2-Gr composite, as well as the high loading of HRP. Therefore, this biosensor is potentially suitable for H2O2 analysis in environmental, pharmaceutical, food or industrial applications.

A general approach using principal component analysis was applied to amperometric data obtained from flow injection analysis (FIA) to select conducting electroactive polymers (CEPs) and applied potential waveforms for discrimination of potassium and methylamine. The results were compared with the selection from the application of the PCA approach for cyclic voltammetry data in our previous research. Good agreement between the two methods of selection was found, which indicates that within the general qualitative limits of the approach, PCA can be applied for selection of chemical and electrochemical parameters for FIA detection/discrimination using CEP sensor arrays detector for a range of analytes.

A novel modified electrode was constructed by the electro-polymerization of 4,5-dihydroxy-3-[(2-hydroxy-5-sulfophenyl)azo]-2,7-naphthalenedisulfonic acid trisodium salt (acid chrome blue K (ACBK)) at a graphene oxide (GO)-nafion modified glassy carbon electrode (GCE). The characterization of an electrochemically synthesized poly-ACBK/GO-nafion film was investigated by electrochemical impedance spectroscopy (EIS), cyclic voltammetry (CV), atomic force microscopy (AFM) and scanning electron microscopy (SEM) techniques, and the results were interpreted and compared at each stage of the electrode construction. Electrochemical oxidation of eight β-agonists – clenbuterol, salbutamol, terbutaline, ractopamine, dopamine, dobutamine, adrenaline, and isoprenaline, was investigated by CV at the different electrodes. At the poly-ACBK/GO-nafion/GCE, the linear sweep voltammetry peak currents of the eight β-agonists increased linearly with their concentrations in the range of 1.0–36.0 ng mL−1, respectively, and their corresponding limits of detection (LODs) were within the 0.58–1.46 ng mL−1 range. This electrode showed satisfactory reproducibility and stability, and was used successfully for the quantitative analysis of clenbuterol in pork samples.

Diffuse reflectance infrared spectra of differently mercerized cotton poplin fabrics are interpreted with the aid of fuzzy clustering and multivariate chemometrics methods (PCA and SIMCA). Fuzzy clustering analysis of spectra from blank, slack, and stretch mercerized samples shows that three clusters can be identified, and this conclusion is supported by the PCA display method and SIMCA classification. Spectra from slack mercerized samples, treated at three different temperatures, are also readily discrim inated by the same three chemometrics methods.

"Catalytic damage" occurs in cotton fabrics during hydrogen peroxide bleaching. The model for catalytic damage proposed previously by Meyer, Kokot, Weber, and Zürcher is compared with a laboratory simulation of cotton cellulose damage produced using electrogenerated oxygen species at metal electrodes. Additional electrochemical information is provided to support the previously proposed mechanism of the damage of a cotton poplin. Diffuse reflectance infrared spectroscopy and chemometrics are used for relative qualitative and quantitative interpretation of the damage.

Treating cotton fabrics with electrogenerated oxygen at a Pt anode provides a lab oratory method for simulating the "catalytic damage" phenomenon. Samples of cotton voile were treated in this manner using different current and temperature conditions to damage the fabric. Diffuse reflectance infrared spectra of a series of these samples treated at 80°C were then analyzed using fuzzy clustering, an unsupervised classification method. The resulting classes were assigned a number (0 to 4) nominally indicating the extent of fabric damage as measured by this spectroscopic technique. This series of spectra together with the damage class numbers was then used to construct a cali bration set by principal components regression. The calibration was successfully val idated with a similar set of samples and also used to predict the relative fabric damage on other oxidatively affected voile samples.

A study of the polarization of copper and mild steel electrodes in the absence and presence of cotton fabric in an alkaline environment has been carried out. In each case passive film formation on the metal substrate is followed by the OER reaction. For those experiments in which the electrodes were in loose contact with the fabric, exhaustion of OH− ion in the solution between the metal substrate and the fabric resulted in a decrease in the rate of the OER. This can be attributed to a change in mechanism from that in an alkaline to that in an acid environment. The interaction of the electrogenerated O2 with the cotton cellulose leads to degradation of the latter; this is comparable to the “catalytic damage” observed during H2O2 bleaching of cellulose. The increased damage observed to the fabric compared to when the O2 is generated on Pt supports the role of both Cu and Fe as catalysts for the O2 cellulose reaction.

Two sets of cotton fabrics—one consisting of different types of fabric and the other of a fabric sampled sequentially during its normal processing stages—were investigated by DRIFT spectroscopy. The band assignments were consistent with previous work but, in general, the spectra could not be differentiated on visual examination. However, they were successfully qualitatively and quantitatively distinguished with the use of chemometrics; a chemical basis for fabric clustering was also indicated. This approach is a significant improvement on previously reported work with KBr disk IR sampling.

Hole formation in cotton fabrics similar to that observed during the peroxide bleaching process and known as "catalytic damage" may be produced by exposing the fabric to an electrochemical process involving generation of oxygen at platinum anodes. A morphological study of an electrochemically damaged poplin fabric is de scribed. Several morphological fiber changes are identified, including crack formation consistent with granular and spiral splittings. A qualitative model is proposed high lighting a possible sequence of morphological changes that occur during oxidation and culminate in fiber rupture.

Polypyrrole was electrochemically deposited onto cotton fabrics with the aid of a water-soluble adhesive. The conductivity and surface structure of the resultant polymer were studied, showing a templated dendritic growth on the surface of the cotton fabric. The mechanism for templated growth is discussed.

The study of kaolinite surfaces is of industrial importance. In this work we report the application of chemometrics to the study of modified kaolinite surfaces. DRIFT spectra of mechanochemically activated kaolinites (Kiralyhegy, Zettlitz, Szeg, and Birdwood) were analyzed using principal component analysis (PCA) and multicriteria decision making (MCDM) methods, PROMETHEE and GAIA. The clear discrimination of the Kiralyhegy spectral objects on the two PC scores plots (400-800 and 800-2030 cm(-1)) indicated the dominance of quartz. Importantly, no ordering of any spectral objects appeared to be related to grinding time in the PC plots of these spectral regions. Thus, neither the kaolinite nor the quartz, are systematically responsive to grinding time according to the spectral criteria investigated. The third spectral region (2600-3800 cm(-1)OH vibrations), showed apparent systematic ordering of the Kiralyhegy and, to a lesser extent, Zettlitz spectral objects with grinding time. This was attributed to the effect of the natural quartz on the delamination of kaolinite and the accompanying phenomena (i.e., formation of kaolinite spheres and water). With the MCDM methods, it was shown that useful information on the basis of chemical composition, physical properties and grinding time can be obtained. For example, the effects of the minor chemical components (e.g., MgO, K(2)O, etc.) indicated that the Birdwood kaolinite is arguably the most pure one analyzed. In another MCDM experiment, some support was obtained for the apparent trend with grinding time noted in the PC plot of the OH spectral region.

Cotton fabrics may be oxidatively bleached and damaged by electro-generated species at metal electrodes. Such fabrics were investigated by DRIFT spectroscopy. The spectra agree well with the literature, although spectra from differently damaged fabrics cannot be readily distinguished. Spectral discrimination is facilitated by principal components analysis, and the electrochemical parameters which control the fabric damage can be successfully predicted by PC regression.

Two different sets of processed cotton fabrics were investigated by FT-IR and FT-Raman spectroscopy. The chemometric technique of principal component analysis, was applied to the IR and Raman spectra from each fabric series in an attempt to discriminate between the various processing stages. The results indicate that a combination of the two techniques and chemometrics adequately discriminates between cotton samples from each processing stage.

A woollen fabric sample has been oxidized by electro-generated oxygen species produced at a platinum electrode. This treatment produced three visually discoloured or bleached regions. The areas of the fabric that were located close to the electrode surface showed dark brown discoloration. On either side of this region, bleaching of the wool was apparent to various degrees. Fabric well removed from the electrode appeared unaffected by the treatment, and was used as a reference. Such samples were analysed by the complementary techniques of FT-IR and FT-Raman spectroscopy, and the pattern recognition method of principal components analysis (PCA). The samples were successfully separated into three groups on the basis of the levels of known oxidation intermediates from cystine and other readily oxidizable amino-acid residues present in wool-keratin.

A DRIFT method for collecting spectra from dye mixtures (50 - 500 ng) extracted from small textile samples (2 mm yarn) is outlined. Results of experiments using library search routines for matching of IR spectra of simple (< 5 components) dye mixtures indicate that matches can be distinguished satisfactorily, however, with complex (8 - 14 components) dye mixture matching of duplicate spectra is less well defined. The application of principal component analysis for matching and discrimination of small dye extracts from a worn garment suggests that this is a useful approach and can add to the TLC information about the sample.© (1992) COPYRIGHT SPIE--The International Society for Optical Engineering. Downloading of the abstract is permitted for personal use only.

The application of scanning densitometry to the analysis of dyes extracted from transferred fibers is examined. The Camag high-performance thin-layer chromatography (HPTLC)/thin-layer chromatography (TLC) scanner can provide all of the information normally available from visual examination of the TLC plates. The position, color, and relative proportions of the various components are obtained in a semiquantitative form. The instrument can provide useful data in both the visible and fluorescence modes with greater sensitivity than is available from visual observations. The potential of the instrument for examination of dyes from pale-colored fibers is demonstrated. The data obtained are objective and do not suffer from the variations that can occur when using subjective visual observations.