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Application of chemometric methods to resolve intermediates formed during photo- catalytic degradation of methyl orange and textile wastewater from Ethiopia
摘要： The efficiency of two catalysts (TiO2 and TiO2 supported on zeolite) for the photocatalytic degradation of methyl orange dye and wastewaters from Ethiopian textile industry was evaluated by chemometric methods from UV/Vis data of the reaction mixtures at different times. Multivariate curve resolution statistical analysis combined with an alternating least squares algorithm (MCR-ALS) proved to be an efficient method to resolve the different intermediates present during the photocatalytic degradation of the pollutants and to provide information about their evolution with time. Methyl orange photodegradation at pH = 3 showed different intermediate and concentration profiles than at pH = 6. The evolution of intermediates from textile wastewater photodegradation could also be resolved by this method. From the concentration profile or the reactants, a kinetic study was done. Results revealed that all the photodegradation reactions followed a first order kinetics. When TiO2 supported in Zeolite is used, reactions are in general slower, probably due to a mechanism of adsorption/desorption.
关键词： Wastewater,Chemometrics,Dye photodegradation,Methyl Orange,MCR-ALS
更新于2025-09-23 15:23:52
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Chemometrics-assisted determination of Sudan dyes using zinc oxide nanoparticle-based electrochemical sensor
摘要： Multivariate curve resolution-alternating least squares (MCR-ALS) assisted with electrochemical techniques was applied for simultaneous determination of Sudan II and III at a surface of zinc oxide nanoparticles (ZnONPs) modified carbon paste electrode. Characterization of the ZnONPs and the nanostructured modified electrode was performed by X-ray diffraction (XRD), scanning electron microscopy (SEM), electrochemical impedance spectroscopy (EIS) and cyclic voltammetry (CV) techniques. Response surface methodology using central composite rotatable design was employed to design of experiments and achieving to optimum values of variables. For simultaneous determination of Sudan II and III, electrochemical second order data were obtained by changing of pulse height in differential pulse voltammetry technique. MCR-ALS was performed on the data to obtain the decomposition peaks of analytes. Then, the detection limits were obtained 1.87 and 2.62 nM for Sudan II and III, respectively. Finally, this method used for the analysis of the two analytes in real samples.
关键词： ZnO nanoparticles,Differential pulse voltammetry,MCR-ALS,Sudan dyes,Second order data,Response surface methodology
更新于2025-09-23 15:22:29
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Portable and benchtop Raman spectrometers coupled to cluster analysis to identify quinine sulfate polymorphs in solid dosage forms and antimalarial drug quantification in solution by AuNPs-SERS with MCR-ALS
摘要： This paper proposes for the first time: (a) a qualitative analytical method based on portable and benchtop backscattering Raman spectrometers coupled to hierarchical cluster analysis (HCA) and multivariate curve resolution – alternating least-squares (MCR-ALS) to identify two polymorphs of antimalarial quinine sulfate in commercial pharmaceutical tablets in their intact forms and (b) a quantitative analytical method based on gold nanoparticles (AuNPs) as active substrates for surface-enhanced Raman scattering (SERS) in combination with MCR-ALS to quantify quinine sulfate in commercial pharmaceutical tablets in solution. The pure concentration and spectral profiles recovered by MCR-ALS proved that both formulation present different polymorphs. These results also were confirmed by two clusters observed in HCA model, according to their similarities within and among the samples that provided useful information about homogeneity of different pharmaceutical manufacturing processes. AuNPs-SERS coupled to MCR-ALS was able to quantify quinine sulfate in the calibration range from 150.00 to 200.00 ng mL-1 even with strong overlapping spectral profile of background SERS signal, proving that is a powerful ultrahigh sensitivity analytical method. This reduced linearity was validated through a large calibration range from 25.00 to 175.00 μg mL-1 used in a reference analytical method based on high performance liquid chromatography with diode array detector (HPLC-DAD) coupled to MCR-ALS for analytical validation purposes even in the presence of coeluted compound. The analytical methods herein developed are fast, because second-order chromatographic data and first-order SERS spectroscopic data where obtained in less than 6 and 2 min, respectively. Concentrations of quinine sulfate were estimated with a low root mean square error of prediction (RMSEP) values and a low relative error of prediction (REP%) in the range 1.8-6.1%.
关键词： Quinine sulfate pharmaceutical tablets,Raman spectrometer,polymorphs,HCA and MCR-ALS,AuNPs-SERS
更新于2025-09-23 15:19:57
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Tracking small heterogeneity in binary mixtures of aliphatic and aromatic hydrocarbons: NIR spectroscopic, 2DCOS and MCR-ALS studies
摘要： To our best knowledge, this is the ?rst spectroscopic study of small heterogeneity at a molecular level in binary mixtures of aliphatic and aromatic hydrocarbons. The composition-dependent spectra of benzene/toluene, benzene/n hexane, benzene/cyclohexane, n hexane/n heptane and n hexane/cyclohexane mixtures were recorded by NIR transmission technique in the whole range of mole fractions. A comprehensive exploration of the experimental data was performed by two-dimensional correlation analysis (2DCOS) and chemometric methods. In addition, we calculated excess NIR molar absorption spectra and parameter of ER, which allows for comparison of the degree of deviation from ideality for various mixtures. Our results reveal that all studied mixtures deviate from the ideal mixture. The extent of these deviations is small for the mixtures were both components are aromatic or aliphatic and increases for aromatic/aliphatic mixtures. In addition, molecular shapes have an important effect on the degree of deviation from the ideal mixture. As expected, benzene/n hexane is the most non-ideal mixture, while behavior of n hexane/n heptane and benzene/toluene mixtures is close to the ideal one. Our results suggest that in the mixtures with the largest deviations from ideality are present homoclusters of both components and heteroclusters. The heteroclusters exist in the whole range of compositions, while the homoclusters appears above a certain concentration limit. If both components of the mixture are similar, the molecules with equal probability form the homo- and heteroclusters. In the case of unlike components, the molecules prefer to form the homoclusters. The homoclusters of both components in the mixture are similar as those observed in bulk constituents. This means that deviation from the ideal mixture results from presence of the heteroclusters.
关键词： Aliphatic/aromatic hydrocarbons,NIR,Clustering,MCR-ALS,Binary mixtures,2DCOS,Chemometrics,Excess absorption spectra,Microheterogeneity
更新于2025-09-19 17:15:36
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Application of infrared spectroscopy as Process Analytics Technology (PAT) approach in biodiesel production process utilizing Multivariate Curve Resolution Alternative Least Square (MCR-ALS)
摘要： Process Analytical Technology means at-line collection of analytical information from the process when the reaction is in progress. Obtained information enables process engineers to better control the Critical Process Parameters and direct the reaction to desirable routs. Near-infrared spectroscopy due to its analytical features, as well as the high capability of automation, versatile sampling and spectral acquisition methods is a useful tool in process monitoring when coupled to chemometrics. The Multiple Scatter Correction preprocessing technique and Alternative Least Square method can extract spectral and concentration information of a reaction mixture simultaneously, were employed pairing with fiber optic Near-Infrared spectroscopy in 1000-2250 nm spectral region was employed to extract the analytical information from the biodiesel production process. The obtained output demonstrated appropriate results about the concentration and type of components during the process. The kinetics of the reaction was also studied using the obtained results and showed a three-stage kinetics with different rates.
关键词： MCR-ALS,Near-Infrared spectroscopy,Process Analytical Technology,Biodiesel
更新于2025-09-19 17:15:36
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Emerging micropollutants determination by NIR spectroscopy using pseudo-univariate calibration and TF-SPME coupled with 96-well plate system
摘要： In this study, an innovative approach was developed to determine simultaneously the emerging micropollutants bisphenol A (BPA), 3-(4-methylbenzylidene) camphor (4-MBC), triclocarban (TCC), benzophenone (BZP) and 2-ethyl-hexyl-4-trimethoxycinnamate (EHMC) in water employing near infrared spectroscopy (NIR) coupled with thin film solid-phase microextraction (TF-SPME) using the chemometric tool of multivariate curve resolution with alternating least squares (MCR-ALS). In addition, a 96-well plate system was employed to increase the analysis throughput of the proposed methodology. Samples were submitted to TF-SPME procedure (previously optimized in previous work to exhibit the best performance for extraction and desorption conditions) and its extracts were analyzed by NIR. A pseudo-univariate calibration model for each analyte was developed by associating the relative concentration obtained using MCR-ALS with the reference concentration (i.e. theoretical concentration). The correlation coefficients obtained were 0.9238, 0.8722, 0.7872, 0.8856 and 0.9128 for BPA, 4-MBC, TCC, BZP and EHMC, respectively. With the use of these pseudo-univariate models, the determination of the analytes exhibited absolute errors lowers than those of the chromatographic technique for BZP and TCC. For BPA, 4-MBC and EHMC the absolute error was lower than 10 μg L-1. This approach can provide a cheap and rapid strategy for the direct quantification of these micropollutants in water samples.
关键词： pseudo-univariate calibration,MCR-ALS,96-well plate,Emerging micropollutants,TF-SPME,NIR
更新于2025-09-19 17:13:59
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Fourier transform infrared imaging and quantitative analysis of pre-treated wood fibers: A comparison between partial least squares and multivariate curve resolution with alternating least squares methods in a case study
摘要： Pretreated lignocellulosic fibers were used as a case study to compare two chemometric methods for the quantification of chemical components in Fourier transformed infrared (FT-IR) images. Partial least squares (PLS) and multivariate curve resolution with alternating least squares (MCR-ALS) methods were applied to the images to quantify glucans, lignin and hemicellulose content. The main problem for calibration in samples from natural origin is to obtain proper reference material for pixel to pixel quantification. Furthermore, chemical components in wood experience changes after different pretreatment conditions; therefore commercially available reference material may not have the same identity of the components present in the sample. Concentration information of bulk samples obtained by wet chemistry methods, along with the median spectrum of whole images, was used as an alternative for PLS calibration in this scenario. Results show that both methods provided similar spatial distribution for lignin and hemicellulose in the concentration maps, but image reconstruction of glucans shows differences in distribution between the two methods. PLS models used to quantify pixels in an image were previously validated through the prediction of global concentration of samples, using the median spectrum of different images (RMSEP ? 1.3% for glucans, 1.0% for lignin and 0.9% for hemicelluloses); The range of pixel concentration predicted in a single image was too narrow possibly due to the lack of a calibration set with a wider dynamic range. Concentration maps obtained with MCR-ALS were satisfactory and the range of concentration for pixels was more consistent with what would be expected. A quantification approach that does not need a calibration set was used to transform concentration profiles into real concentration units for pixels. Therefore MCR-ALS was a more suitable method for quantification in this specific case study.
关键词： PLS,Lignocellulosic fibers,Hyperspectral imaging,Quantitative analysis,MCR-ALS
更新于2025-09-12 10:27:22