Reflectance Fourier Transform Infrared Spectroscopy Research Articles

Enhancing forensic investigations: Identifying bloodstains on various substrates through ATR-FTIR spectroscopy combined with machine learning algorithms

The forensic analysis of bloodstains on various substrates plays a crucial role in criminal investigations. This study presents a novel approach for analyzing bloodstains using Attenuated Total Reflectance Fourier Transform Infrared spectroscopy (ATR-FTIR) in combination with machine learning. ATR-FTIR offers non-destructive and non-invasive advantages, requiring minimal sample preparation. By detecting specific chemical bonds in blood components, it enables the differentiation of various body fluids. However, the subjective interpretation of the spectra poses challenges in distinguishing different fluids. To address this, we employ machine learning techniques. Machine learning is extensively used in chemometrics to analyze chemical data, build models, and extract useful information. This includes both unsupervised learning and supervised learning methods, which provide objective characterization and differentiation. The focus of this study was to identify human and porcine blood on substrates using ATR-FTIR spectroscopy. The substrates included paper, plastic, cloth, and wood. Data preprocessing was performed using Principal Component Analysis (PCA) to reduce dimensionality and analyze latent variables. Subsequently, six machine learning algorithms were used to build classification models and compare their performance. These algorithms comprise Partial Least Squares Discriminant Analysis (PLS-DA), Decision Trees (DT), Logistic Regression (LR), Naive Bayes Classifier (NBC), Support Vector Machine (SVM), and Neural Network (NN). The results indicate that the PCA-NN model provides the optimal solution on most substrates. Although ATR-FTIR spectroscopy combined with machine learning effectively identifies bloodstains on substrates, the performance of different identification models still varies based on the type of substrate. The integration of these disciplines enables researchers to harness the power of data-driven approaches for solving complex forensic problems. The objective differentiation of bloodstains using machine learning holds significant implications for criminal investigations. This technique offers a non-destructive, simple, selective, and rapid approach for forensic analysis, thereby assisting forensic scientists and investigators in determining crucial evidence related to bloodstains.

Differentiation and prediction of the in vitro antifungal activity of Brazilian propolis against Fonsecaea pedrosoi using chemometrics and diffuse reflectance infrared Fourier Transform spectroscopy

The in vitro antifungal activity of ethanolic extracts of propolis was evaluated at five different concentrations in twelve Fonsecaea pedrosoi strains using agar dilution. Eight propolis extracts were collected from towns located in the central region of the state of Rio Grande do Sul, Brazil. Diffuse reflectance infrared Fourier Transform spectroscopy (DRIFTS) was employed to analyze the spectra of lyophilized propolis extracts. The use of chemometric tools allowed for the development of models with more relevant factors and with fewer variables. Partial least squares (PLS) regression was applied, allowing for the development of PLS-DRIFTS models to predict antifungal activity of all fungal strains with root mean square error of cross validation (RMSECV) lower to 5.00 mm2 and coefficient correlation of cross-validation (R2) upper to 0.99 with five to eight latent variables at 4000-2400 and 2200-600 cm-1. Concluding, DRIFTS models associated with chemometrics are powerful screening tools of propolis samples with fungistatic properties against Fonsecaea pedrosoi.

Plasma-Induced Interfacial Processes in Metal Halides FTIR Gas Cell Windows

Fourier transform infrared spectroscopy (FTIR) is one of the most widely used vibrational diagnostic techniques to investigate gas-phase reactive oxygen and nitrogen species (RONS). However, the technique carries intrinsic challenges, particularly in relation to interfering peaks in the spectral data. This study explores the interfacial processes that occur when reactive oxygen and nitrogen species generated by a non-equilibrium air plasma interact with the metal halide windows of an FTIR gas cell, leading to the appearance and evolution of spurious absorption peaks which complicate spectral interpretation. Raman spectroscopy, X-ray photoelectron spectroscopy, time of flight secondary ion mass spectrometry and attenuated total reflectance-FTIR spectroscopy were used to elucidate the origin of spurious absorption peaks spanning the 1400–1300 cm−1 spectral range as a result of KBr exposure to plasma generated species. It was found that plasma exposed KBr contained a lower atomic fraction of Br which was replaced by the NO3 nitrate group, the main absorbance peak of which progressively evolved with plasma exposure and affected the window transparency over the corresponding FTIR region. A correlation was revealed between KNO3 formation, plasma power and exposure time to a growth and change in molecular vibrational energies corresponding to asymmetric NO3 stretching vibrations in the KNO3 structure.

Interaction mechanisms of typical collectors with zircon surfaces and their influence on surface morphology and hydrophobicity for selective flotation

Zircon is the primary mineral that contains the critical metals zirconium and hafnium. However, the extraction of pure zircon from its natural ore is challenging. The inadequate understanding of the interaction mechanisms between traditional flotation collectors, namely n-octyl phosphonic acid (nOPA), octyl-hydroxamic acids (OHA), and oleic acid (OL), with zircon, has hindered the development of highly selective flotation reagents. Therefore, a combination of atomic force microscopy (AFM), X-ray photoelectron spectroscopy (XPS), Diffuse Reflectance Infrared Fourier Transform Spectroscopy (DRIFTS), Zeta potential tests, contact angle measurements, and flotation tests was employed to elucidate the mechanism of collector adsorption on surface morphology and the chemical bonding interactions at the interface. The AFM, XPS, and DRIFTS results consistently demonstrate that all three reagents can chemically bond with zircon surfaces. nOPA exhibits stronger interactions with zircon compared to OL and OHA, as it coordinates with two zirconium sites to form a monolayer. Zeta potential and contact angle measurements reveal that the surface morphology and weak adsorption, which is driven by weak interactions, contribute to an improvement in hydrophobicity. Flotation results further validate that the three reagents can selectively float zircon in specific pH ranges. The interfacial bonding interactions, which are influenced by weak interactions, play significant roles in the flotation of zircon.

Determination of the pKa Value of Protonated Mono and Polyamine in Solution Using Fourier Transform Infrared Titration.

The pKa values of propanolamine hydrochloride (PAMH) and poly(allylamine hydrochloride) (PAAMH) in concentrated solutions were determined by both Fourier transform infrared spectroscopy (FT-IR) titration and classical potentiometric (POT) titration and compared. Starting with the respective fully protonated forms PAMH and PAAMH and increasing the pH value by sodium hydroxide addition in situ attenuated total reflection FT-IR (ATR FT-IR) spectra on PAMH and PAAMH solutions show the variation of diagnostic infrared (IR) bands. From the decrease of the most intense δ(NH3+) band the dissociation process of the NH3+ groups could be followed. Thereby, from the respective normalized band area A the dissociation degree αIR of the ammonium groups could be determined. Plotting pH versus αIR and fitting this curve by a modified Henderson-Hasselbalch function pH = pKa + B log (αIR/1 - αIR) the parameters pKa and cooperativity factor B were obtained. pKa values from FT-IR titration were qualitatively in line with respective pKa values from POT titration. Quantitative systematic pKa deviations between polyelectrolyte (PEL) and respective monoelectrolyte and the tentative effects of PEL molecular weight, ambient ionic strength, and titration concept (FT-IR and POT) are discussed based on classical models of weak PEL.

Enhancement of Fe-Nb interaction by acid modification over SO42--FeOx-Nb2O5 catalyst for NH3 selective catalytic reduction of NOx

A series of iron-based composite oxide catalysts, modified with acid and niobium, were produced for the purpose of selective catalytic reduction of NOx with NH3 (NH3-SCR) via co-precipitation. The obtained SO42--FeOx-Nb2O5 (S-FeNbOx) catalyst exhibited significantly better SCR performance than the unmodified FeOx catalyst, with a NOx conversion above 90% and N2 selectivity higher than 95% in the temperature range of 275–450 °C. The characterization results suggest that the addition of Nb not only modifies the electronic structure and alleviates the reducibility but also enhances the surface acidity of the catalysts. The sulfuric acid modification of FeOx-Nb2O5 catalyst promotes the formation of redox-acid sites. The in situ Diffuse Reflectance Infrared Fourier Transform spectroscopy (DRIFTs) results revealed that the combining sulfuric acid and niobium modifications resulted in a significant increase in the amount of Brønsted acid sites, and also led to a blue shift of the band related to the Lewis acid sites, implying the existence of a synergistic effect of the two modification methods. The creation of redox-acid sites significantly enhances the adsorption and activation capacity of NH3 on the catalyst surface. These results suggest that the NH3-SCR reaction to primarily follow the Eley-Rideal (E-R) mechanism on the catalyst.

UV Light Causes Structural Changes in Microplastics Exposed in Bio-Solids.

Bio-solids (biological sludge) from wastewater treatment plants are a significant source of the emission of microplastics (MPs) into the environment. Weakening the structure of MPs before they enter the environment may accelerate their degradation and reduce the environmental exposure time. Therefore, we studied the effect of UV-A and UV-C, applied at 70 °C, on three types of MPs, polypropylene (PP), polyethylene (PE), and polyethylene terephthalate (PET), that are commonly found in sewage sludge, using three shapes (fibers, lines, granules). The MPs were exposed to UV radiation in bio-solid suspensions, and to air and water as control. The structural changes in and degradation of the MPs were investigated using Attenuated Total Reflectance-Fourier Transform Infrared Spectrometry (ATR-FTIR) and surface morphology was performed with SEM analysis. UV exposure led to the emergence of carbonyl and hydroxyl groups in all of the PP samples. In PE and PET, these groups were formed only in the bio-solid suspensions. The presence of carbonyl and hydroxyl groups increased with an increasing exposure time. Overall, UV radiation had the greatest impact on the MPs in the bio-solids suspension. Due to the surface-to-volume ratio of the tested samples, which influences the degradation rate, the fibers were more degraded than the other two plastic shapes. UV-A was slightly more effective at degrading the MPs than UV-C. These findings show that ultraviolet radiation in combination with an elevated temperature affects the structure of polymers in wastewater bio-solids, which can accelerate their degradation.

Utilizing Drug Amorphous Solid Dispersions for the Preparation of Dronedarone per os Formulations

Dronedarone (DRN), an antiarrhythmic drug, exhibits potent pharmacological effects in the management of cardiac arrhythmias. Despite its therapeutic potential, DRN faces formulation challenges due to its low aqueous solubility. Hence, the present study is dedicated to the examination of amorphous solid dispersions (ASDs) as a strategic approach for enhancing the solubility of DRN. Initially, the glass forming ability (GFA) of API was assessed alongside its thermal degradation profile, and it was revealed that DRN is a stable glass former (GFA III compound) that remains thermally stable up to approximately 200 °C. Subsequently, five commonly used ASD matrix/carriers, i.e., hydroxypropyl methylcellulose (HPMC), povidone (PVP), copovidone (PVP/VA), Soluplus® (SOL), and Eudragit® E PO (EPO), were screened for the formation of a DRN-based ASD using film casting and solvent shift methods, along with miscibility evaluation measurements. SOL proved to be the most promising matrix/carrier among the others, and, hence, was used to prepare DRN ASDs via the melt-quench method. The physicochemical characterization of the prepared systems (via pXRD) revealed the complete amorphization of the API within the matrix/carrier, while the system was physically stable for at least three months after its preparation. In vitro release studies for the ASDs, conducted under non-sink conditions, revealed the sustained supersaturation of the drug for at least 8 h. Finally, the use of attenuated total reflectance (ATR) FTIR spectroscopy showed the formation of a strong molecular interaction between the drug molecules and SOL.

Lattice-Strained Metallic Aerogels as Efficient and Anti-Poisoning Electrocatalysts for Oxygen Reduction Reaction.

Lattice strain engineering optimizes the interaction between the catalytic surface and adsorbed molecules. This is done by adjusting the electron and geometric structure of the metal site to achieve high electrochemical performance, but, to date, it has been rarely reported on anti-poisoned oxygen reduction reaction (ORR). Herein, lattice-strained Pd@PdBiCo quasi core-shell metallic aerogels (MAs) were designed by "one-pot and two-step" method for anti-poisoned ORR. Pd@PdBiCo MAs/C maintain their original activity (1.034 A mgPd -1 ) in electrolytes with CH3 OH and CO at 0.85 V vs. reversible hydrogen electrode (RHE), outperforming the commercial Pd/C (0.156 A mgPd -1 ), Pd MAs/C (0.351 A mgPd -1 ), and PdBiCo MAs/C (0.227 A mgPd -1 ). Moreover, Pd@PdBiCo MAs/C also show high stability and anti-poisoning with negligible activity decay after 8000 cycles in 0.1 m KOH+0.3 m CH3 OH. These results of X-ray photoelectron spectroscopy, CO stripping, and diffuses reflectance FTIR spectroscopy reveal that the tensile strain and strong interaction between different elements of Pd@PdBiCo MAs/C effectively optimize the electronic structure to promote O2 adsorption and activation, while suppressing CH3 OH oxidation and CO adsorption, leading to high ORR activity and anti-poisoning property. This work inspires the rational design of MAs in fuel cells and beyond.

Heterogeneous reactivity of soybean/palm biodiesel soot with NO2 and CF3COOH in a Knudsen reactor and DRIFTS/TGA/SEM characterization of the soot

The characteristics and atmospheric reactivity of soot generated from an alternative fuel (soybean/palm biodiesel) have been investigated for the first time using a Knudsen flow reactor with a mass spectrometer as detector for gaseous species. The heterogeneous reactions with nitrogen dioxide (NO2) and trifluoroacetic acid (CF3COOH, TFA) have been investigated. Uptake coefficients calculated for the reaction of NO2 (γ0= (3.85 ± 0.70) ∙10–3) are one order of magnitude higher than the corresponding TFA reactions (γ 0= (6.06 ± 0.24) ∙10–4). NO is the only product observed in the gas phase. Knudsen cell reactor has also been used in the characterization of chemical functions on the surface since NO2 can be used to identify reducing groups, while TFA is used to evaluate basic sites. Compared to other soot samples, biodiesel soot shows higher reactivity with NO2 which has implications in the regeneration process of the diesel particulate filter (DPF). IR bands attributable to polycyclic aromatic compounds have been observed by Diffuse Reflectance Infrared Fourier Transform spectroscopy (DRIFTs). Bands of carbonyl compounds are also clearly observed. Thermogravimetric analysis/ differential scanning calorimetry-mass spectrometry (TGA/DSC-MS) is used to obtain more information about the volatile organic compounds present on the soot surface. Scanning Electron Microscopy/Energy Dispersive Spectroscopy (SEM/EDS) analysis indicates a particle size in the range 14–40 nm and carbon as the major element (92 %). According to the obtained results, a mechanism of processes occurring at the surface has been proposed.

Insights into the Sensing Mechanism of a Metal-Oxide Solid Solution via Operando Diffuse Reflectance Infrared Fourier Transform Spectroscopy.

Recently, the influence of Nb addition in the oxide solid solution of Sn and Ti was investigated with regard to the morphological, structural and electrical properties for the production of chemoresistive gas sensors. (Sn,Ti,Nb)xO2-based sensors showed promising features for ethanol monitoring in commercial or industrial settings characterized by frequent variation in relative humidity. Indeed, the three-metal solid solution highlighted a higher response level vs. ethanol than the most widely used SnO2 and a remarkably low effect of relative humidity on the film resistance. Nevertheless, lack of knowledge still persists on the mechanisms of gas reaction occurring at the surface of these nanostructures. In this work, operando Diffuse Reflectance Infrared Fourier Transform spectroscopy was used on SnO2- and on (Sn,Ti,Nb)xO2-based sensors to combine the investigations on the transduction function, i.e., the read-out of the device activity, with the investigations on the receptor function, i.e., compositional characterization of the active sensing element in real time and under operating conditions. The sensors performance was explained by probing the interaction of H2O and ethanol molecules with the material surface sites. This information is fundamental for fine-tuning of material characteristics for any specific gas sensing applications.

Infrared Spectroscopy Study of Edge Water Penetration at Hydrophilic Bonding Interface

In this article, we report on the use of a new characterization technique to measure the water penetration at the bonding interfaces and to quantify it. This complements previous studies done using X-ray reflectometry and surface acoustic microscopy: Fourier Transform Infra-Red Multiple Internal Reflection (FTIR-MIR) spectroscopy is used here to characterize the evolutions of contributions of silanols, surface bonded water and free liquid water groups.

Novel porous ambient temperature cured fly ash geopolymer for lead adsorption from wastewaters

ABSTRACT This paper discusses the ability of the fly ash (FA) and abmbient cured Alkali activated Fly ash geopolymer (FAAG) for sequestering Pb (II) ions from aqueous solution. Various physiochemical properties such as the influence of pH and contact time were investigated for achieving the conditions for maximum removal via batch mode using powdered samples. The adsorbents were characterized by employing powder X-Ray diffraction, Attenuated Total Reflection Fourier Transform Infra-Red spectroscopy, and Scanning Electron Microscopy/EDAX before and after the treatment. The adsorption capacity of Pb2+ ions by raw FA and FAAG were examined by the Inductively coupled plasma mass spectrometry (ICP-MS). The results represented that the maximum adsorption capacity of Pb2+ ions by FAAG is 75 mg/g with attained equilibrium time of 120 min whereas raw fly ash at 150 min at 21.5 mg/g capacity. The pozzolanic reactivity of fly ash in water glass hardening resulted mainly N-A-S-H gel and traces of lead silicate due to the immobilization of lead in the network. This was conformed from the binding energy lines at 139.7 eV in XPS survey lines and lead silicate at 25 and 34° 2θ as identified in XRD phase assemblages. ICP-MS test results of leachate of lead immobilized geopolymer sample are devoid of lead ions and thus sorption sites of fly ash geopolymer lead to potential safety disposal of lead. Thus, recycling of fly ash into geopolymer by less energy intensive process and subsequent use in heavy metal disposal could achieve the concept of disposal waste and recycling, which could contribute to achieve the sustainable goals.

Calcium oxide nanoparticles: Biosynthesis, characterization and photocatalytic activity for application in yellow tartrazine dye removal

Dyes are substances that have a high polluting potential, due to their low biodegradability and chemical stability, causing serious environmental damage when disposed of incorrectly. Yellow tartrazine (YT) dye as an environmental liability requires attention, since it causes toxic effects in fish (Danio rerio) with a potential allergic effect in humans. In this context, the present study aims to synthesize and characterize calcium oxide nanoparticles (CaO-NPs) to evaluate the photocatalytic activity for the YT photodegradation under visible irradiation. CaO-NPs were synthesized by the biosynthesis method from golden linseed (Linum usitatissimum L.) extract. Central Composite Rotational Design (CCRD 23) was used to determine the ideal condition for the photocatalytic tests. X-ray diffraction (XRD), zeta potential (ZP), physical adsorption of N2, zero charge point (pHzcp), Attenuated Total Reflectance Fourier Transform Infrared Spectroscopy (ATR-FTIR), Scanning Electron Microscopy by Energy Dispersive Spectroscopy (SEM-EDS), Diffuse Reflectance Spectroscopy (DRS) and Field Emission Gun – Scanning Electron Microscope (FEG-SEM) were used to the CaO-NPs characterization. Thus, CaO-NPs presented SBET = 14±0.02 m2g−1, Dp = 20.9±0.02 nm and Vp = 0.054±0.004 cm3g−1, characteristic of a mesoporous material. ATR-FTIR spectrum showed characteristic stretches of specific functional groups (–CH, –CO, C = C, Ca-O, –OH) from plant extract and metallic precursor. CaO-NPs showed pHZCP equal to 7.74, positive surface charge (+12.7 mV) and bang gap energy of 2.61 eV. FEG-SEM micrographs showed that has a small agglomeration with defined morphology, but with irregular particle size (around 48 nm), and SEM-EDS micrographs showed an elemental composition (in weight) of the 50.24% oxygen, 3.32% magnesium, 2.29% iron, 10.44% calcium, 14.07% silicon, 3.33% aluminum and 0.63% potassium. Regarding CCRD 23, the ideal condition was the pH = 7.0, [CaO-NPs] = 1.2 g/L and [YT] = 20 mg/L, with 76.2% of photodegradation and a pseudo first-order reaction specific reaction rate k = 0.089 min−1. After V cycles of CaO-NPs recycling, there was a decrease of around 22.83%, indicating a saturation of the active sites available in the nanocatalyst Therefore, CaO-NPs showed potential application for TY photodegradation to be used in wastewater treatment being an alternative nanocatalyst, meeting nanotechnology and sustainable development.

Effect of applied standard wood machining fluid on colour and chemical composition of the machined wood surface

Appropriate monitoring of wood machining processes is a key issue to ensure the expected quality of the processed wood, expected efficiency and minimize energy consumption of production processes. A new trend is the design of environmentally friendly machining fluids. In this paper, as a preliminary study in this field, the effect of applied standard wood machining fluid on changes in the colour and chemical composition of the machined wood surface is presented. Scots pine wood (Pinus sylvestris L.) was used for this research. Colour measurements were carried out based on the three-axis CIELab system test in time intervals and coefficients such as: colour chroma (Cab*), colour saturation (Sab*), colour hue (h°), and total colour changes (ΔE*). Changes in chemical composition were analysed on the Attenuated Total Reflectance Fourier Transform Infrared Spectroscopy (ATR FT-IR). The results confirmed that standard machining fluids cause a significant change in the colour of the treated pine surface, which decreases over time but is still present even after 24 h. For the spectral analysis, no chemical changes were observed between the machining fluid and the wood. However, the fluid particles remained in the wood after 24 h. In order to reduce the effect of the machining fluid on the colour of the wood, its composition should be changed to allow and/or accelerate the evaporation of their components from the treated wood surface.

Effects of highland barley protein and β‐glucan addition on the flour structure, bread quality and starch digestibility of whole wheat bread

SummaryWhole wheat bread is rich in nutrition, but its starch digestibility is unsatisfactory. Thus, how to reduce its digestibility has attracted much attention. This study investigated the effects of highland barley protein and β‐glucan on the pasting properties, and thermal properties of whole wheat flour to reveal the mechanism of highland barley protein and β‐glucan regulating the in vitro digestibility. The digestibility results showed that β‐glucan and protein could slow down starch digestion to some degree. The cross‐section structure determination results indicated that β‐glucan and protein decreased the porosity. The differential scanning calorimetry and thermogravimetric analysis results showed that β‐glucan and protein increased the onset of pasting, decreased the peak temperature and enthalpy of pasting and decreased the thermal stability. The Attenuated Total Reflectance Fourier Transform Infrared Spectroscopy results revealed a blue‐shift in the ‐OH position of the bread added with protein and β‐glucan (from 995.59 to 996.07 cm−1), indicating that the hydrogen bonding might form intramolecularly. In this study, the addition of highland barley protein and β‐glucan was proved to be helpful in decreasing the in vitro digestibility and showed modification in the texture quality of bread, which might be suitable for diabetic patients.

Efficacy Comparison of Three Atmospheric Pressure Plasma Sources for Soybean Seed Treatment: Plasma Characteristics, Seed Properties, Germination

Plasma seed treatment has proven to be a useful technique for improving germination, growth dynamics, as well as plant resistance. In this paper, we studied the efficacy of soybean seeds treatment using various sources of cold atmospheric pressure plasma generated in air. We compared three types of plasma treatments: direct treatment with plasma generated by a diffuse coplanar surface barrier discharge (DCSBD), direct treatment with plasma generated by a multi-hollow surface dielectric barrier discharge, and indirect treatment using the gaseous products of plasma generated by an air plasma jet. The composition of plasma generated by each of the sources was analysed using optical emission spectroscopy and Fourier Transform Infrared spectroscopy (FTIR). Parameters of the plasma treatments have been optimized to improve soybean germination. Plasma-treated seeds were examined by the means of water contact angle, surface free energy and imbibition measurements, attenuated total reflectance FTIR (ATR-FTIR), x-ray photoelectron spectroscopy (XPS) and scanning electron microscope (SEM) analyses. Surface analysis by ATR-FTIR and XPS showed changes in the chemical bonds on the surface of the plasma-treated seeds, which led to an increase in wettability and imbibition. SEM analysis confirmed that the plasma treatment is non-invasive and does not cause changes in seed surface morphology. Among the studied sources, DCSBD proved to be the best suited for soybean seed treatment in terms of germination improvement as well as treatment time and energy efficiency.

Plasma Polymerization of Precipitated Silica for Tire Application.

Pre-treated silica with a plasma-deposited (PD) layer of polymerized precursors was tested concerning its compatibility with Natural Rubber (NR) and its influence on the processing of silica-silane compounds. The modification was performed in a tailor-made plasma reactor. The degree of deposition of the plasma-coated samples was analyzed by ThermoGravimetric Analysis (TGA). In addition, Diffuse Reflectance Infrared Fourier Transform spectroscopy (DRIFTs), X-ray Photoelectron Spectroscopy (XPS), and Transmission Electron Microscopy (TEM) were performed to identify the morphology of the deposited plasma polymer layer on the silica surface. PD silica samples were incorporated into a NR/silica model compound. NR compounds containing untreated silica and in-situ silane-modified silica were taken as references. The silane coupling agent used for the reference compounds was bis-(3-triethoxysilyl-propyl)disulfide (TESPD), and reference compounds with untreated silica having the full amount and 50% of silane were prepared. In addition, 50% of the silane was added to the PD silica-filled compounds in order to verify the hypothesis that additional silane coupling agents can react with silanol groups stemming from the breakdown of the silica clusters during mixing. The acetylene PD silica with 50% reduced silane-filled compounds presented comparable properties to the in-situ silane-modified reference compound containing 100% TESPD. This facilitates processing as lower amounts of volatile organic compounds, such as ethanol, are generated compared to the conventional silica-silane filler systems.

External Reflection FTIR Spectroscopy Applied to Archaeological Pottery: A Non-Invasive Investigation about Provenance and Firing Temperature

The mineralogical composition of archaeological pottery is closely related to the raw material and the firing conditions, thus constituting a source of information both on the origin and the manufacturing technology of ceramic artefacts. The techniques used to clarify the composition of the ceramic material from the point of view of the mineralogical phases include X-ray diffraction (XRD), Fourier-transform infrared spectroscopy (FTIR) and petrographic analysis. Such techniques normally require the taking of a sample from the object, thus often limiting their applicability to sherds rather than intact vessels. The present study aims to investigate the possibility of applying reflection FTIR spectroscopy in the mid- and near-IR to the non-invasive analysis of the mineralogical composition of archaeological pottery, with reference to a set of Etruscan ceramic materials from the excavation of Tarquinia (Italy).

Goat milk powders enriched with grape pomace seed extract: Physical and techno-functional properties

This study aimed to evaluate the physical (particle size and ζ-potential) and techno-functional properties (emulsifying and foaming) of goat milk powders enriched with grape pomace seed extract (TME), as promising food ingredients in the formulation of functional food. Attenuated Total Reflectance Fourier Transform Infrared (ATR-FTIR) and Raman spectroscopies, along with advanced chemometric tools were employed as well as Scanning Electron Microscopy (SEM) for analyzing TME powders. All powders exhibited a unimodal particle size distribution and ζ-potential values more negative than −36 mV. ATR-FTIR and Raman spectroscopies combined with principal component analysis (PCA) demonstrated distinct separation among skimmed goat milk (M), thermally treated skimmed goat milk (TM), and TME powders in different spectral regions (amide I, II, III, and fingerprint region). This separation resulted from the applied thermal treatment, the presence of phenolic compounds and their complexes with goat milk proteins, and the formation of Maillard reaction products. SEM analysis confirmed the different morphology and shapes of M, TM and TME powders. The 0.1% solutions of M, TM and TME exhibited good emulsifying properties (emulsion activity index and emulsion stability index) but showed poor foaming properties, except for the M sample. Solution concentrations higher than 0.1% for all samples (0.5% and 1.0%) displayed poor techno-functional properties. In summary, a schematic representation of the arrangement of casein micelles in 0.1% M, TM and TME samples, on oil/water and air/water surfaces was provided. The production of TME powders represents an innovative strategy for waste recovery in the production of functional food ingredients with good emulsifying properties.