Francisco Bosch Reig

Francisco Bosch Reig
University of Valencia | UV · Analytical Chemistry

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141
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Publications (141)
Article
Two asymptotic constant ratio methods applied to the quantification of individual components of solid samples using attenuated total reflectance-Fourier transform infrared spectroscopy (ATR-FTIR) and X-ray diffraction (XRD) are described. The methods involve the measurement of the peak current/peak areas of selected signals (diffraction peaks in XR...
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A theoretical model to determine the concentration of an analyte in the presence of unknown interferents using spectral-type data is described. The method involves absorbance measurements at three wavelengths and the calculation of specific absorbances yielding a hyperbolic relationship between absorbance ratios and analyte concentrations. The conc...
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A method for quantifying the individual components of mineral samples based on attenuated total reflectance – Fourier transform infrared spectroscopy (ATR-FTIR) is described, extending the constant ratio (CR) method to analytes absorbing in a common range of wavenumbers. Absorbance values in the spectral region where the analytes absorb relative to...
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A web-based database of voltammograms is presented for characterizing artists' pigments and corrosion products of ceramic, stone and metal objects by means of the voltammetry of immobilized particles methodology. Description of the website and the database is provided. Voltammograms are, in most cases, accompanied by scanning electron microphotogra...
Research
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The color of 7 types of Spanish unifloral honey from rosemary,orange biosson, lavender, eucalyptus, sunflower, and honeydew was investigated for is potential use a characterization parameter. Color were estimated by visual comparison with a Lovibond 1000 instrument, the readings of which were transformed into Plund units.
Research
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Oil and fats start descomposing from the moment theyare isolated fromtheir natural enviroment.. The descomposition products formedup to 300ºC were determined by means of H-NMR spectroscopy and an FTIR spectroscopic method.
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The use of the scanning electrochemical microscopy (SECM) technique for identifying and mapping both organic and inorganic pigments in sub-microsamples from pictorial specimens is described. This methodology, inspired in the voltammetry of immobilized particles technique, permits the study of textural properties of paint layers and mapping the dist...
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A solid-state electrochemical application of the H-point standard addition method (HPSAM) for quantifying two electroactive compounds, A, B, that produce strongly overlapped voltammetric peaks is described. It is based on peak current measurement in square-wave voltammograms recorded for solid samples containing a reference compound R, upon additio...
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A solid-state electrochemical application of the H-point standard addition method to the quantification of two depositable metals A and B, which produce strongly overlapped stripping peaks, is described. The method is based on the mechanical transference of mixtures of the solid sample plus a selected compound, of a reference depositable metal R, a...
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A HPLC-fluorescence method for characterization of proteinaceous glues from binding media used in pictorial works of art prior to conservation or restoration treatment is proposed. Fluorescence derivatization of amino acids released by acid hydrolysis of standard proteins is studied. The derivatization reagent was o-phtalaldehyde with 2-mercaptoeth...
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A study attempted to characterize natural waxes used in pictorial works of art was carried out by means of gas chromatography. The analytical treatment requires prior hydrolysis of the waxes to release the fatty acids (FA) (myristic (myr), palmitic (pal), oleic (ole), stearic (ste), araquidic (ara), behenic (beh), lignoceric (lig), cerotic (cer)) f...
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In the present work, a study attempting to characterize the Manila elemi and Mexican copal resins from the Burseraceae family, which are used as components of varnishes and binding media of artworks, has been carried out. A new GC-MS method involving the use of methyl chloroformate as derivatisation reagent has been proposed. A second method which...
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Electrochemical identification of natural insoluble curcuma and safflower dyes in microsamples usable for microchemical examination of works of art and archaeological artifacts via solid state voltammetry is described. Upon attachment to paraffin-impregnated graphite electrodes in contact with aqueous acetate and phosphate buffers, curcuma and saff...
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A HPLC-fluorescence method for identification of drying oils from binding media or protective film used in pictorial works of art prior to conservation or restoration is proposed. Fluorescence derivatization of fatty acids released by hydrolysis of structural drying oils is studied. The derivatization reagent was 4-(bromomethyl)-7-methoxycoumarin w...
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A new HPLC-UV-Vis method for identification of drying oils from binding media or protective film used in pictorial works of art prior to conservation or restoration is proposed. Chromophore derivatization of fatty acids released by hydrolysis of structural drying oils is studied. The derivatization reagent selected was 2-nitrophenylhydrazine with 1...
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A method for quantitatively determining the relationship boron/lead in ceramic materials is presented. It is based on the attachment of microsamples of ceramic frits to an electrochemical quartz crystal microbalance (EQCM). After a reductive deposition step in the −0.25 to −0.85 V (vs. AgCl/Ag) potential range, well-defined stripping peaks are reco...
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Characterization of ox bile, traditionally used in painting, is of interest in the fields of archaeometry and conservation and restoration of works of art. Bile acids, fatty acids (F), and cholesterol found in ox bile have been identified using a derivatization method that combines the formation of ethyl esters from the carboxylic groups and the tr...
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A method to suppress the interference of pigments in the analysis of proteinaceous media used in paintings is presented in this paper. This method is based on the formation of metallic ion-ethylenediaminetetraacetic acid (EDTA) complexes previous to the derivatisation process, using ethyl chloroformate (ECF), to transform the amino acids in N(O,S)-...
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A derivatisation method that combines the formation of ethyl esters from the carboxylic groups and trimethylsilyl ethers from hydroxyl groups of the components of diterpenic resins is presented in this paper. This methodology involves two experimental steps: (1) formation of ethyl esters using ethyl chloroformate; and (2) the esterified compounds a...
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A method for quantitatively determining boron in minerals and ceramic materials is described. It is based on the abrasive attachment of mixtures of ZnO plus sample to PIGEs. After a reductive deposition step, square wave voltammograms recorded for those modified electrodes immersed into 0.10 M NaCl+0.25 M mannitol provide well-defined stripping pea...
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A method for identifying Co, Cu, Sb, Sn, Fe, Zn, and Zr pigments in glasses using square-wave voltammetry as the detection mode is described. It is based on the abrasive attachment of glass microsamples to graphite/polyester composite electrodes. Sample amounts less than 1 μg are used allowing for the study of archaeological samples. In all cases w...
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This work is the archaeometric study of different types of materials used in iron production in the Iberian Period (6th-2nd century b.c.). The materials were recovered in several archaeological digs (which makes it possible to date the archaeological remains) on different sites in the Levante area of the Iberian Peninsula. The samples selected for...
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Two stopped-flow manifolds have been proposed for individual or simultaneous determination of chromium and cobalt in water samples. Automated procedures based on multicommutation systems have emphasised the differences of their catalytic effect in luminol–hydrogen peroxide chemiluminescence reaction. A more rapid decay of signal was observed for Co...
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The generalised H-point standard addition method (GHPSAM) was applied to quantify phenol and o-cresol in waters and compared with other analytical approaches. The method is based on spectroscopic and kinetic measurement of the formation of derivatives with p-aminophenol and KIO(4) in presence of NaOH. First, pseudo-first order kinetic behaviour of...
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An electrochemical method for identifying anthraquinone-type dyes in microsamples from works of art, based in the voltammetry of microparticles approach, is reported. Upon attachment onto graphite/polyester composite electrodes, natural pigments aloe, henna, cochineal red, madder lake, kermes, shellac, and alizarin and purpurin taken as reference m...
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This work is the archaeometric study of the different types of materials recovered in the same excavation or archaeological dig (which makes it possible to accurately date the remains found) on the island of Ibiza (Spain). The samples found belong only to the phase of iron forging and span a very wide historical period from the 6th to the 18th cent...
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The simultaneous determination of chromium and cobalt in water samples has been studied. Chemiluminescence registers based on the luminol–hydrogen peroxide reaction have obtained by a batch procedure. PLS algorithms have employed to model the time-response (formation and destruction of emitter). The influence of the presence of two metals and the n...
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A methodology for quantifying calcium carbonate (875 and 712 cm(-1)) and silica (798 and 779 cm(-1)) by FTIR spectroscopy applying the constant ratio method is proposed. The studied method is applied for quantitative analysis of calcite and quartz in geological samples. The suggested method uses potassium ferricyanide (2115 cm(-1)) as standard and...
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A method for determining the iron(III)/iron(II) ratio in ceramic materials based on microsample attachment to graphite/polyester composite electrodes is presented. This quotient is of considerable interest for determining the nature and firing conditions of the original materials in archaeological ceramics. The electrochemistry of iron in ceramic m...
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An in-depth chemical-analytical study has been performed on biscuit and mortar from 17th-18th century tiles from a mediaeval hermitage in the province of Valencia (Spain). Representative samples were chosen from the tile fragments available, using appearance, essentially color and consistency, as the criterion. The chemical composition was analyzed...
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This paper reports an analytical study of enamel on fragments of medieval tiles using atomic spectroscopy techniques — AAS, XRF and SEM/EDX. The samples came from a hermitage in the region of Valencia (Spain) and have different motifs, mainly floral ones in a wide variety of colors. A study of the soluble salts in the biscuits and mortar was carrie...
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In this work, we present the results obtained in an analytical study of the different types of proteinaceous binding media most commonly used in paintings, using GC-FID as the technique of analysis and GC-MS as a confirmatory technique. The application of this methodology requires prior hydrolysis of the proteins in the binding media to obtain free...
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The electrochemical response of metal ions in different samples of coloured ceramic tin-lead glazes attached to graphite/polyester composite electrodes is described. In addition to the ubiquous signals for lead, reductive dissolution processes are followed by anodic stripping peaks for Co, Cu, Sb, Mn, Sn and Fe, enabling the direct identification o...
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This paper is an analytical study of the possibility of applying the linear range of the substitution-dilution method to correct the matrix effect in quantitative analysis by X-ray fluorescence (XRF) spectroscopy. The analytical range is obtained from a series of samples prepared in the form of glass discs by substituting the unknown sample with a...
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Multivariate calibration is tested as an alternative to model chromium(III) concentration versus chemiluminescence registers obtained from luminol-hydrogen peroxide reaction. The multivariate calibration approaches included have been: conventional linear methods (principal component regression (PCR) and partial least squares (PLS)), nonlinear metho...
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Differentiation between the synthetic polymers used in former restorations of works of art and the original materials used by the artist is of great interest; such differentiation is needed to establish an adequate process of restoration for the work of art. A specific method of sample preparation based on a filtration and deposition-evaporation se...
Article
Multivariate calibration is tested as an alternative to model chromium(III) concentration versus chemiluminescence registers obtained from luminol-hydrogen peroxide reaction. The multivariate calibration approaches included have been: conventional linear methods (principal component regression (PCR) and partial least squares (PLS)), nonlinear metho...
Article
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Direct standardization (DS) and piecewise direct standardization (PDS) methods are applied to multivariate standardization of chemiluminescence signals using PLS model as the calibration model.The linear concentration interval of the chemiluminescence determination was determined. This interval was located using univariate robust calibration by lea...
Article
Direct standardization (DS) and piecewise direct standardization (PDS) methods are applied to multivariate standardization of chemiluminescence signals using PLS model as the calibration model.The linear concentration interval of the chemiluminescence determination was determined. This interval was located using univariate robust calibration by lea...
Article
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The electrochemical response of different iron pigments attached to graphite–polyester composite electrodes is described. Characteristic differential pulse voltammetric profiles were obtained for green earth, iron oxide red, Mars black, ochre yellow, Sienna raw, umber raw and Van Dyke brown. Proton-assisted reductive dissolution processes occur at...
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The present study proposes a new flow cell called a bundle cell for chemiluminescence analysis. The results obtained were compared with those achieved by manual and automated batch procedures and flow manifolds with different cells: an common quartz flow cell, a helix cell and the most used spiral cell. Figures of merit such as limit of detection,...
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The influence of the presence and the type of pigments in the lipid binding media of paintings were studied by gas chromatography with flame ionization detector. The drying oils were linseed stand oil, poppy oil and sunflower oil, and the pigments studied were cadmium red, cobalt blue, tin white, lead white, chalk and plaster of Paris, commonly use...
Article
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A new method, based on the combined use of scanning electron microscopy-x-ray microanalysis, Fourier transform infrared spectroscopy, gas chromatography and differential pulse voltammetry, is proposed which permits a parallel investigation of organic and inorganic materials and the characterization of the artistic technique employed in canvas paint...
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The alteration of copper pigments in art samples was studied by linear scan and cyclic voltammetry using sample-modified Elvacite 2044 film electrodes on the basis of two-dimensional diagrams of charge transfer coefficients calculated from Tafel plots of reductive dissolution processes vs. peak potential. Characteristic voltammetric peaks were obta...
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GC-FID was used as single methodology for the identification and differentiation of proteins, lipids and ox bile from binders used in artistic paintings. The samples were hydrolyzed by HCl. Subsequently, the simultaneous formation of volatile derivatives of the amino, fatty and bile acids with ethyl chloroformate was performed quickly and safely in...
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The generalized H-point standard-additions method (GHPSAM) is proposed in order to obtain the phenol concentration in water samples when the matrix is completely unknown. The procedure involves solid-phase extraction in BondElut PPL cartridges and data handling of the UV-visible spectrophotometry measurements. The spectral regions where the unknown...
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A mathematical model based on the dilution–addition method (DAM) for multi-elemental analysis using an X-ray fluorescence technique is proposed. The conditions for sample preparation do not require both the unknown and standard samples to be similar in composition and mineralogy, and the unknown sample is replaced quantitatively by the standard sam...
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The present paper deals with the selection of variables for the H-point and generalised H-point standard additions methods (HPSAM and GHPSAM, respectively). Both methods are applied for the resolution of spectroscopic interfered signals in the UV-vis range. The HPSAM is a suitable method for the resolution of binary and ternary mixtures when the in...
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A method is proposed for boron determination in ceramic materials, boracic raw materials and ceramics frits of different compositions by wavelength dispersive X-ray fluorescence technique. The instrumental conditions were studied and the sample preparation procedures were optimized. The reference method used was the potentiometric titration of mann...
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The H-point curve isolation method (HPCIM) for the detection of unknown interferences in chromatography is proposed. The method allows one to estimate the UV-vis spectra of interfering species in a sample as well as to test the purity of the chromatographic peaks. Besides the detection of the unknown interferences in a sample, this method allows on...
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This paper shows how the generalized H-point standard-additions method (GHPSAM) can be used to obtain the total concentration or concentrations of different chemical forms of an analyte when the matrix of the sample is completely unknown. The spectral regions where the interferent behaviour can be considered as linear are found and the analyte conc...
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The generalized H-point standard-additions method (GHPSAM) is used in order to obtain the total Cr(VI) and chromate concentration in water samples whose matrices are completely unknown. Moreover, a new methodology, which is a modification of the GHPSAM, is proposed for the simultaneous determination of the two major chemical forms of Cr(VI) present...
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Inorganic pigments in paintings and polychromed sculptures are studied by cyclic voltammetry and differential pulse stripping voltammetry using micro-sample coatings in Paraloid B72-film modified electrodes. Characteristic cathodic and anodic differential pulse profiles were obtained in the +0.4 to −1.0 V vs. SCE potential range for different cadmi...
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Direct identification of lead(II) and (IV) in glazed ceramics by cyclic voltammetry and differential pulse voltammetry is described. Characteristic cathodic and anodic profiles are obtained for microsample coatings in Paraloid B72-film electrodes immersed in NaCl and HAc/NaAc media. The electrochemical response of PbO, PbO2 and Pb3O4, and a series...
Article
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The oxidative deterioration of polyunsaturated fatty acids (PUFAs) in culinary oils and fats during episodes of heating associated with normal usage (80-300 degrees C, 20-40 min) has been monitored by Fourier transform infrared spectroscopy (FTIR). The thermal oxidation of PUFAs is a free radical chain reaction, in which hydroperoxides are generall...
Article
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The generalised H-point standard addition method (GHPSAM) is proposed for isolating the analytical signal of an analyte from the signal of an unknown sample. Samples containing two and three coeluting compounds have been analysed. The accuracy of the predictions depends on the shape of the analyte and interferent spectra but not on the degree of ch...
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A systematic study is performed about several factors involved in the measurements when a absorbent blank is used, as molar absorption coefficient of the formed complex, absorbance of the blank at the measured wavelength, and kind of spectrophotometer used (conventional double-beam or diode-array). It is proved that the usual methodology, measuring...
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A method for the simultaneous spectrophotometric determination of calcium and magnesium in mineral waters with an FIA system is tested. The method is based on the reaction between the analytes and arsenazo(III) at pH 8.5. The calculations of the amounts of both analytes in the samples are carried out with the H-point standard addition method (HPSAM...
Article
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An analytical methodology to quantify compounds in complex mixtures by FTIR spectroscopy is proposed and the “Constant Ratio Method” (CRM) was developed. The addition of a standard to the sample allows us to establish a constant KMS characteristic of the Analyte/Standard system which can be employed as a quantification factor of the analyte in . In...
Article
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The oxidative deterioration of culinary oils and fats during episodes of heating associated with normal usage (80°C–300°C, 20–40 min) was monitored by FTIR spectroscopy. The thermal oxidation of polyunsaturated fatty acids during heating was studied by the determination of unsaturation percentage and trans isomers at various temperatures and heatin...
Article
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Oils and fats start decomposing from the moment they are isolated from their natural environment. Heating accelerates oxidative rancidity and frying at high temperatures produces thermal degradation with the formation of decomposition products, such as aldehydes, ketones, free acids and hydroxilic compounds that in high levels can be harmful to hum...
Article
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A study by FT-IR spectroscopy which aims to compare the stability of five polymers, Araldit XW396/XW 397, Vitralit 7256, Loctite 350, Desmodur N 75/Viacryl SM 564/65 and Krafft silicone commonly used in the restoration of archaeological glass objects when subjected to thermal ageing, UV light ageing and cyclic ageing in SO2 pollutant chamber has be...
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A comparison between the different proposed methods to perform the standard addition in an on-line way (flow injection analysis) is made. The different assemblies (reverse and conventional FIA) and the employed standards in every method are compared. Three analyses were carried out, two of them were analyses of samples of pH indicators (methylorang...
Article
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The method described is based on the selection of a wavelength in the sample spectrum that is called ‘reference wavelength’, all measured wavelengths are previously assayed in order to select this reference wavelength. Several wavelengths can be used as the reference. The interferent spectrum is calculated as a function of the interferent absorbanc...
Article
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Cefotaxime was derivatised with 1,2-naphthoquinone-4-sulphonate (NQS), extracted into solid-phase cartridges (C18) and detected using a UV-visible detection system. Optimum conditions for this new procedure were: hydrogencarbonate-carbonate buffer, pH 10.5, 5-min reaction time at 25 degrees C and an NQS concentration of 7.1x10(-3) mol l(-1). The ac...
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This paper establishes the fundamentals of the H-point standard additions method (HPSAM) and generalized H-point standard additions method (GHPSAM) in the flow injection technique. Two kinds of analytical signals can be employed, FIA peaks and spectra. Different analytical problems have been studied: determinations of one analyte in the presence or...
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The present report shows how to derivatize cephalexin with 1,2-naphthoquinone-4-sulphonate (NQS) into solid-phase extraction cartridges (C18) using UV–visible detection. Optimum conditions for this new procedure are: hydrogen carbonate/carbonate buffer pH=10.5, 5 min reaction time at 25°C and NQS concentration of 7.1×10−3 mol l−1. The accuracy and...
Article
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A mathematical addition–dilution model for matrix correction was applied to the determination of iron(III), potassium and sulfur oxides in an industrial cement by XRF. The samples were prepared in the form of pellets. A cement of known composition was used as a single multi-element standard and the compactant and diluent was mannitol. The intensiti...
Article
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To ascertain the most discriminant variables for seven types of Spanish commercial unifloral honeys, stepwise discriminant analysis was performed. Fifteen parameters [pH; water content; electrical conductivity; x, y, and L, chromatic coordinates from the CIE-1931 (xyL) color space; fructose; glucose; sucrose; maltose; isomaltose; maltulose; kojibio...
Article
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An improvement in the way to locate linear spectral intervals for unknown interferents which overlap the analyte signal in UV–visible spectrophotometry is offered as an alternative to the method previously described by Campíns-Falcó et al. (Anal. Chim. Acta, 302, 323 (1995)). In that report, quotients of the second-derivative spectra of the sample...
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This paper presents analysis of Valencian paintings from the fourteenth to the seventeenth century, to provide a scientific study of the development of this style of painting and innovations in painting technique. Four altarpieces representing this period have been examined. Microscopical, SEM-EDX and XRD techniques have been used to identify the s...
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The levels of various sugars (fructose, glucose, sucrose, maltose, maltulose, kojibiose, isomaltose, raffinose, erlöse and melezitose) as well as the glucose/fructose and glucose/water ratios were determined in different Spanish unifloral honey types (rosemary, orange blossom, lavender, sunflower, eucalyptus, heather, honeydew). Sugars were determi...