0000000000023580
AUTHOR
M. Luisa Cervera
A comparative study on sample preparation procedures for supplementary foods by ICP-OES: Green chemistry considerations
An inductively coupled plasma optical emission (ICP-OES) method was developed for the simultaneous determination of major, minor and trace elements in food. Preliminary studies focused on selecting suitable operational conditions in order to provide the highest sensitivity and to maximize the number of analytes to be determined without spectral or matrix interference. Ruthenium and rhenium were evaluated as internal standards and samples were analyzed at different dilution levels. Furthermore, a comparative study was carried out by using three sample digestion methods, microwave-assisted digestion with HNO3/H2O2, dry ashing and dry ashing with Mg(NO3)2/MgO as an ashing aid. Adequate precisi…
Determination of total mercury in nuts at ultratrace level
Abstract Total mercury, at μg kg−1 level, was determined in different types of nuts (cashew nut, Brazil nuts, almond, pistachio, peanut, walnut) using a direct mercury analyser after previous sample defatting and by cold vapour atomic fluorescence spectrometry. There is not enough sensitivity in the second approach to determine Hg in previously digested samples due to the strong matrix effect. Mercury levels in 25 edible nut samples from Brazil and Spain were found in the range from 0.6 to 2.7 μg kg−1 by using the pyrolysis of sample after the extraction of the nut fat. The accuracy of the proposed method was confirmed by analysing certified reference materials of Coal Fly Ash-NIST SRM 1633…
Room temperature acid sonication ICP-MS multielemental analysis of milk
Abstract Room temperature acid sonication of milk samples is proposed as a fast alternative methodology for the determination of the total content of 45 elements (Li, Al, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, As, Se, Rb, Sr, Y, Mo, Ag, Cd, In, Sn, U, Sb, Te, Cs, Ba, Hg, Pb, Bi, Th, La, Ce, Pr, Nd, Sm, Eu, Gd, Dy, Ho, Er, Tm, Yb, Lu, Hf and Ta) in milk by inductively coupled plasma mass spectrometry (ICP-MS). The aforementioned procedure involves a 10 min sample pre-treatment. Measurements were made in quantitative and semiquantitative (Totalquant ® ) modes of analysis using Rh as internal standard and Be, Ge, Tb and Re for internal calibration of the equipment in the semiquantitative mode. The…
Non-chromatographic speciation analysis of arsenic and antimony in milk hydride generation atomic fluorescence spectrometry
Abstract A rapid, high sensitivity method has been developed for the determination of As(III), As(V), Sb(III) and Sb(V) in milk samples by using hydride generation atomic fluorescence spectrometry. The method is based on the leaching of As and Sb from milk through the sonication of samples with aqua regia followed by direct determination of the corresponding hydrides both before and after reduction with KI. It was confirmed by recovery experiments on spiked commercially available samples that neither the reduced nor the oxidized forms of the elements under study or mixtures of the two oxidation states were modified by the room temperature sample treatment with aqua regia. The methodologies …
On-line speciation of mercury in fish by cold vapour atomic fluorescence through ultrasound-assisted extraction
A fully mechanized procedure has been developed for the speciation of mercury in fish samples by using cold vapour atomic fluorescence spectrometry (CV-AFS). Sample slurries in an acid mixture in the presence of a surfactant and with traces of K2Cr2O7, were injected into a flow system, sonicated and merged with 1 ml of an oxidant mixture of KBr/KBrO3 heated at 50 °C in a water bath and total Hg determined by CV-AFS. Sonicated sample slurries were also measured, in the absence of KBr/KBrO3, in order to obtain a second series of data which could be employed to establish the concentrations of free Hg(II). Different compositions of the acidic extractant solutions were evaluated by mixing HCl, H…
Mineral profile of kaki fruits (Diospyros kaki L.)
The main objective of this study was the determination of the mineral profile of 167 kaki fruit (Diospyros kaki L.) samples produced from different regions of Spain, including samples with the protected designation of origin (PDO) 'Kaki Ribera del Xúquer' Valencia (Spain). Samples were analysed by inductively coupled plasma optical emission spectroscopy (ICP-OES) and inductively coupled plasma mass spectrometry (ICP-MS). Consumption of one piece of kaki fruit (200-400 g) would give a mineral intake providing 1-10% of the recommended daily allowance (RDA) for calcium, 1-30% for copper and potassium, 1-15% from iron and magnesium, up to 1% of sodium, and up to 4% of zinc. ANOVA analysis indic…
Altered elemental profile as indicator of homeostatic imbalance in pathogenesis of oral submucous fibrosis
Oral submucous fibrosis (OSF) is a potential precancerous condition of the oral cavity and oropharynx. The etiopathogenesis of this complex precancerous condition is still obscure. In addition to deleterious oral habits, malnutrition, and possible genetic predisposition, altered bioelemental status is also likely to play an important role in its pathogenesis. The present study analyzed 68 elements by inductively coupled plasma-mass spectroscopy in oral mucosa of normal and OSF individuals and some interesting alterations in elemental profile in the diseased tissue have been noted, indicating a homeostatic imbalance. These bioelemental alterations leading to homeostatic imbalance might be co…
Speciation of selenium and tellurium in milk by hydride generation atomic fluorescence spectrometry
A simple, fast and highly sensitive method has been developed for the differentiation of Se and Te into their (IV) and (VI) oxidation states in milk samples by HG-AFS. This procedure involves a previous leaching of milk slurries by sonication with aqua regia for 10 min. Se(IV) and Te(IV) were determined by analysis of the samples without a pre-reduction step; being total Se and Te determined after reduction with KBr. The method provides limit of detection values (LOD) of 0.012 and 0.023 ng ml−1 for Se(IV) and Te(IV) respectively. Average relative standard deviation values of 10.5%, 3.9%, 12% and 12.5% were found for the determination of Se(IV), Se(VI), Te(IV) and Te(VI) in milk samples cont…
Determination of As, Sb, Se, Te and Bi in milk by slurry sampling hydride generation atomic fluorescence spectrometry
A simple and fast analytical procedure has been developed for the determination of As, Sb, Se, Te and Bi in milk samples by hydride generation atomic fluorescence spectrometry (HG-AFS). Samples were treated with aqua regia for 10min in an ultrasound water bath and pre-reduced with KBr for total Se and Te determination or with KI and ascorbic acid for total As and Sb, the determination of Bi being possible in all with or without pre-reduction. Slurries of samples, in the presence of antifoam A, were treated with NaBH(4) in HCl medium to obtain the corresponding hydrides, and AFS measurements were processed in front of external calibrations prepared and measured in the same way as samples. Re…
Direct determination of minerals in human diets by infrared spectroscopy and X-ray fluorescence
The use of near and mid infrared spectroscopy and X-ray fluorescence (XRF) to determine the concentration of mineral elements in Spanish human diets was investigated. Thirty-five commercial baby foods, 6 children fast food menus and 13 university canteen menu samples were analysed by infrared and XRF spectroscopy and spectra evaluated by using reference data obtained by inductively coupled plasma optical emission spectroscopy (ICP-OES). Models for calcium, potassium, iron, magnesium, sodium and zinc determination were built and validated. Spectra were pre-treated by using different pre-processing algorithms (multiplicative scatter correction, standard normal variation, first derivate, ortho…
Mineral analysis of human diets by spectrometry methods
Abstract Mineral element determination in human diets is very important for human health, due to the presence in foods of essential and toxic elements or their incorporation in the manipulation and cooking food process. Different instrumental techniques have been used to determine mineral elements in human diets, but atomic spectroscopy and mass spectrometry based ones are the most commonly employed. Sampling procedures for diet analysis are the main critically step for mineral element determination, being employed different standardised protocols. This review summarised critically the state-of-the-art of mineral analysis in human diets, considering sampling, sample preparation and determin…
Determination of thallium in water samples
Abstract This article illustrates the developments of effective preconcentration techniques and highly sensitive detection methods for accurate measurements of Tl species at extremely low concentration in aqueous solutions. The literature on this topic was taken from the Analytical Abstracts in the period 1990–2005.
Removal of Fe(III) from synthetic wastewater into raw and modified clay: Experiments and models fitting
Water pollution by heavy metal ions has become a serious environmental issue especially due to their toxicity and tendency to bioaccumulation. Natural smectite clay was treated using sulfuric acid ...
Atomic fluorescence determination of inorganic arsenic in soils after microwave-assisted distillation
Abstract An inexpensive microwave-assisted distillation procedure has been developed for quantitative determination of inorganic arsenic in soils by atomic fluorescence spectrometry (AFS). After reduction of As(V) to its trivalent state with potassium iodide, inorganic arsenic was distilled as AsCl 3 that was finally determined by atomic fluorescence after hydride generation with NaBH 4 in HCl medium. The different parameters that control the distillation: concentration and volume of HCl, time of distillation, sample weight, and oven load, were studied. The methodology developed has a detection limit of 0.015 μg l −1 , which corresponds to a concentration of 0.006 μg of As per gram of soil,…
Determination of arsenic and antimony in milk by hydride generation atomic fluorescence spectrometry
Abstract A highly sensitive procedure has been developed for total arsenic and antimony determination in milk samples by hydride generation atomic fluorescence spectrometry after microwave-assisted sample digestion. The discrete introduction of 2 ml of digested sample in the automated continuous flow hydride generation system allows us to reduce drastically the sample and HCl consume and to determine several elements from a same sample digestion. The method provides detection limits of 0.006 and 0.003 ng ml−1, a sensitivity of 2390 and 2840 fluorescence units per ng ml−1 for As and Sb respectively, and average relative standard deviation of 2.3% for As and 4.8% for Sb. The analysis of cow m…
A Review on Molybdenum Determination in Solid Geological Samples
This review highlights the necessity for the development of proper sampling and storage, fast pretreatment methodology followed by highly sensitive detection for the determination of molybdenum in geological samples. Distribution of concentration and chemical speciation of molybdenum analysis in solid geological matrices have also been discussed.
Speciation of methylmercury in market seafood by thermal degradation, amalgamation and atomic absorption spectroscopy
Sample thermal decomposition followed by mercury amalgamation and atomic absorption has been employed for the determination of methylmercury (MeHg) in fish. The method involves HBr leaching of MeHg, extraction into toluene, and back-extraction into an aqueous l-cysteine solution. Preliminary studies were focused on the extraction efficiency, losses, contaminations, and species interconversion prevention. The limit of detection was 0.018µgg(-1) (dry weight). The intraday precision for three replicate analysis at a concentration of 4.2µgg(-1) (dry weight) was 3.5 percent, similar to the interday precision according to analysis of variance (ANOVA). The accuracy was guaranteed by the use of for…
Non-chromatographic speciation of toxic arsenic in vegetables by hydride generation-atomic fluorescence spectrometry after ultrasound-assisted extraction.
A non-chromatographic, sensitive and simple analytical method has been developed for the determination of toxic arsenic species in vegetable samples by hydride generation-atomic fluorescence spectrometry (HG-AFS). As(III), As(V), dimethylarsinic acid (DMA) and monomethylarsonic acid (MMA) were determined by hydride generation-atomic fluorescence spectrometry using a series of proportional equations. The method is based on a single extraction of the arsenic species considered from vegetables through sonication at room temperature with H(3)PO(4) 1 mol L(-1) in the presence of 0.1% (w/v) Triton XT-114 and washing of the solid phase with 0.1% (w/v) EDTA, followed by direct measurement of the co…
Multicommutation as an environmentally friendly analytical tool in the hydride generation atomic fluorescence determination of tellurium in milk.
The aim of this study is to show the advantages of the emerging multicommutation methodology based on the use of solenoid valves for Te determination in milk by hydride generation atomic fluorescence spectrometry (HG-AFS). The delivery of a series of alternating sequential insertions of small volumes of samples and reagents gives rise to new hydrodynamic processes and exciting analytical potentials by controlling the time of flow through the on/off-switched solenoid valves. This drastically reduces the reagent consumption by a factor of 4 and the generation of effluents (590 mL h(-1) instead of 750 mL h(-1) generated by the continuous-mode measurement) and also provides an improvement in th…
Hydride generation atomic fluorescence spectrometric determination of ultratraces of selenium and tellurium in cow milk
Abstract A sensitive procedure has been developed for selenium and tellurium determination in milk by hydride generation atomic fluorescence spectrometry (HG-AFS) after microwave-assisted sample digestion. The method provides sensitivity values of 1591 and 997 fluorescence units ng−1 ml−1 with detection limits of 0.005 and 0.015 ng ml−1 for Se and Te, respectively. The application of the developed methodology to the analysis of cow milk samples of the Spanish market evidenced the presence of concentration ranges from 11.1 to 26.0 ng ml−1 for Se, and from 1.04 to 9.7 ng ml−1 for Te having found a good comparability with data obtained after dry-ashing of samples.
Authentication of protected designation of origin artichokes by spectroscopy methods
Abstract Artichoke samples with the protected designation of origin (PDO) ‘Alcachofa de Benicarlo’ were discriminated from those produced in other towns surrounding Valencia and Murcia, outside the PDO frame. Inductively coupled plasma (ICP-OES), near infrared (NIR) and X-ray fluorescence (XRF) were assayed in order to achieve a correct sample classification of the three different origin sample groups (Benicarlo, Valencia and Murcia). Chemometrics was used to compare the ability of classification of artichoke from their origin by using concentration data of mineral elements, determined by ICP-OES, NIR spectra and XRF spectra. Multivariate analysis tools, as principal component analysis (PCA…
Non-chromatographic speciation of toxic arsenic in fish
Abstract A rapid, sensitive and economic method has been developed for the direct determination of toxic species of arsenic present in fish and mussel samples. As(III), As(V), dimethylarsinic acid (DMA), and monomethylarsonic acid (MMA) were determined by hydride generation–atomic fluorescence spectrometry using a series of proportional equations without the need of a chromatographic previous separation. The method is based on the extraction of arsenic species from fish through sonication with HNO3 3 mol l−1 and 0.1% (m/v) Triton and washing of the solid phase with 0.1% (m/v) EDTA, followed by direct measurement of the corresponding hydrides in four different experimental conditions. The li…
On-line bidirectional electrostacking of chromium(III) and chromium(VI) for flame atomic absorption spectrometry determination
Abstract An on-line bidirectional electrostacking-flow injection-flame atomic absorption spectrometry method has been developed for the simultaneous separation, pre-concentration and determination of Cr(III) and Cr(VI). The electrostacking-flow injection unit was established, the pH and components of the support buffer and sample medium were investigated. Results indicated that the ionic mobility, electric field strength and sample area cross-section are the main influence factors on the electrostacking. The calibration range for both, Cr(III) and Cr(VI), was from 20 to 400 μg l −1 . The limit of detection was 7 μg l −1 for three-times the standard deviation of blank values using a electros…
Study of the factors influencing the bioaccessibility of 10 elements from chocolate drink powder
Abstract A risk/benefit assessment of chocolate drink powder has been conducted by evaluating the total contents and the bioaccessibilities of Al, Ba, Cd, Cr, Cu, Fe, Mg, Mn, P and Zn. The bioaccessibility was studied considering the type of sample (traditional, light, diet and organic) and the different factors that may affect it, including physical-chemical parameters of the human digestive process (gastric pH, concentration of bile salts and presence of lipase) and the presence of dietary components (phytate, pectin, cellulose and tannin). The bioaccessibility varied greatly according to the sample type, being greater in the diet and organic samples, and on the element being considered (…
Analytical techniques for the determination of bismuth in solid environmental samples
Abstract Bismuth is a trace element of the Earth’s crust, which is becoming environmentally significant. Although bismuth has relatively low toxicity, it can form characteristic intracytoplasmatic inclusions. This article illustrates the increasing need for fast pre-treatment techniques and highly sensitive detection methods for accurate measurements of bismuth at extremely low concentrations in solid environmental matrices.
Authentication of the protected designation of origin horchata de Valencia through the chemometric treatment of mineral content
Spanish horchata de chufa samples were authenticated based on the determination of mineral elements by inductively coupled plasma atomic emission spectrometry (ICP-OES) combined with different chemometric methods. The ability of multivariate analysis, such as principle components analysis (PCA), classification and regression trees (CARTs) and discriminant analysis (DA) were evaluated in order to achieve a correct sample classification. It was possible to clearly differentiate homemade and long-life commercial samples by all three methods and CART and DA provided an excellent tool to establish the growth origin of the tiger nuts. CART analysis employed the concentration of Mg to discriminate…
Mineral profile of Spanish commercial baby food.
Commercial baby foods are an important part of the daily intake of babies from 6 to 12 months. The mineral profile of commercial baby foods in Spain was determined to establish levels of essential and non-essential elements, and their contribution to adequate intake (AI) and estimated average requirement (EAR). Thirty-five jars of commercial foods containing meat, fish, vegetables and fruit were obtained from the Spanish market and the mineral composition determined for 14 elements. In general, the baby foods analysed were sufficient for an adequate mineral intake, but contributions to AI and EAR for iron, zinc and calcium were very low (5-20%, 10-60% and 10-70%, respectively). This deficie…
Atomic fluorescence determination of total and inorganic arsenic species in beer
A simple and nearly direct procedure has been developed for the determination of As in beers, based on hydride generation and atomic fluorescence detection. Using 2 mol l−1 HCl with a carrier flow of 6 ml min−1, 3% m/v NaBH4 with a flow of 1.3 ml min−1, a reaction coil of 200 cm and an argon flow of 400 ml min−1, total arsenic in beer could be determined in samples diluted 1∶10 with a final concentration of 2 mol l−1 HCl, 1% m/v KI and 0.08% v/v of an antifoam agent. For the estimation of AsIII and AsV concentrations in beer samples, the difference between the analytical sensitivities of the fluorescence signals obtained for As hydride, without and with previous treatment of samples with KI…
Ultrasonic nebulization inductively coupled plasma optical emission spectrometry method for wine analysis
Abstract A methodology was developed to determine mineral elements in wines using Inductively Coupled Plasma Optical Emission Spectrometry combined with ultrasonic nebulization. The concentration of 36 elements (Al, B, Ba, Bi, Ca, Cd, Ce, Co, Cr, Dy, Er, Eu, Fe, Gd, K, La, Lu, Mg, Mn, Mo, Na, Nd, Ni, Pb, Pr, Sb, Sc, Sm, Sr, Tb, Ti, Tm, V, Y, Yb, and Zn) was determined in 59 wine samples and used to distinguish between Brazilian and Spanish wines. The best conditions for the plasma were selected using a two-level factorial design: radiofrequency power 1500 W; plasma gas flow rate 15 L min−1; auxiliary 0.70 L min−1; and nebulizer 0.40 L min−1. An exploratory multivariate analysis by Principal…
Management of tannery wastewaters: treatment of spent chrome tanning bath and vegetable tanning effluents
Abstract In this work, a chain of treatment processes was proposed and described in order to reach better management of mineral and vegetable tannery wastewaters. First, chromium was precipitated from the spent chrome tanning bath by sodium hydroxide (NaOH) and then reformulated to form a complex of basic chromium sulfate which was tested successfully in mineral tanning process. On the other hand, the supernatant recovered after precipitation of chromium with NaOH was used to dilute vegetable tanning wastewaters characterized by a high concentration of polyphenols (about 2,574 mg/L). Diluted effluent was then treated by liming and tangential microfiltration using a ceramic membrane based on…
Cold vapour atomic fluorescence determination of mercury in milk by slurry sampling using multicommutation
Abstract A highly sensitive mechanized method has been developed for the determination of mercury in milk by atomic fluorescence spectrometry (AFS). Samples were sonicated for 10 min in an ultrasound water bath in the presence of 8% (v/v) aqua regia, 2% (v/v) antifoam A and 1% (m/v) hydroxilamine hydrochloride, and after that, they were treated with 8 mmol l −1 KBr and 1.6 mmol l −1 KBrO 3 in an hydrochloric medium. Atomic fluorescence measurements were made by multicommutation, which provides a fast alternative in quality control analysis, due to the easy treatment of a large number of samples (approximately 70 h −1 ), and is an environmentally friendly procedure, which involves a waste ge…
Mineral soil composition interfacing archaeology and chemistry
Abstract In the last decade, different soil types have been analysed to evaluate the effect of human activities from an archaeological point of view. In particular, in the last few years, tremendous advances have been made in sample preparation and analytical methods used in archaeological soil analyses. However, there is still a need to set standardized protocols to achieve different archaeological goals. Therefore, in this study, the analytical methods available to study archaeological soils have been reviewed together with a critical discussion on the challenging archaeological questions, which could be answered by determining their mineral composition. Data on trace elements and rare ea…
Literature survey of on-line elemental speciation in aqueous solutions.
The literature about the on-line speciation in water has been comprehensively studied. Critical examination of this subject reveals that a great deal of work has been performed in this area for inorganic metal species and some organic compounds. The topic studied mainly includes the speciation of chromium, selenium, copper, arsenic, lead, cadmium, mercury, iron, aluminium, nickel, tin, antimony, phosphorus, nitrogen and others. The present literature survey includes also comments about the possibilities and problems of speciation as a function of analytical steps, general strategies involved and methods proposed in the literature for each element or a series of elements.
A preliminary approach to mineral intake in the Spanish diet established from analysis of the composition of university canteen menus
Abstract The concentration of mineral elements in complete menus has in Spain been determined in order to establish the levels of essential and toxic elements and their contribution to the maximum recommended intake. Thirteen university canteen menus obtained from the Burjassot campus, in Valencia, were analysed to establish a first approach on mineral composition in the Spanish diet. The menus were composed of a mixture of cereals, meat, fish, vegetables, fruits and dairy products. Samples were crushed, homogenized and lyophilized, and 25 elements were determinated by inductively coupled plasma optical emission spectroscopy (ICP-OES) after digestion of samples in a microwave oven. Menu sam…
Development of a non-chromatographic method for the speciation analysis of inorganic antimony in mushroom samples by hydride generation atomic fluorescence spectrometry
Abstract A simple and sensitive method has been developed for the direct determination of toxic species of antimony in mushroom samples by hydride generation atomic fluorescence spectrometry (HG AFS). The determination of Sb(III) and Sb(V) was based on the efficiency of hydride generation employing NaBH 4 , with and without a previous KI reduction, using proportional equations corresponding to the two different measurement conditions. The extraction efficiency of total antimony and the stability of Sb(III) and Sb(V) in different extraction media (nitric, sulfuric, hydrochloric, acetic acid, methanol and ethanol) were evaluated. Results demonstrated that, based on the extraction yield and th…
Metal speciation in biological fluids — a review
The literature on the speciation of metal ions in biological fluids is comprehensively reviewed. Critical examination on this subject reveals that major work has been done in blood and urine. Speciation in materials like milk has not yet been widely studied. On the other hand, only few references could be found on sweat, saliva, cell lysate, cerebrospinal, seminal, tear and bronchoalveolar fluids. The topics studied for these fluids were mainly the speciation of arsenic, mercury, aluminium and selenium. Work on the speciation of other elements like zinc, chromium, cadmium, lead, copper, iron etc. have also been carried out in such matrices. The present literature survey includes also a crit…
An Overview of Green Analytical Techniques in the Spectrometric Analysis of Environmental and Biological Samples
ABSTRACT This literature survey presents in a nutshell different parameters for the effectiveness of the green spectrometric procedures, which have been applied to the determination of organics, inorganics, and metal ions in different matrices. The following issues were considered: the main aspects of miniaturization, reagent replacement, reduction of wastes, and on-line recovery and detoxification, which made the analytical procedures sustainable. Also, a discussion of analytical characteristics along with spectrometric methodologies and applications is included.
Determination of chromium(III) and chromium(VI) in mineral water by bidirectional electrostacking and electrothermal atomic absorption spectrometry
Abstract A feasibility investigation was carried out on the use of bidirectional electrostacking for simultaneous separation and pre-concentration of Cr(III) and Cr(VI) and their electrothermal atomic absorption spectrometry (ETAAS) determination. The bidirectional electrostacking manifold was improved, and the effects of sample tube cross-section and electrostacking time on the pre-concentration factor were investigated. Results indicate that the sample tube cross-section and electrostacking time are the main influence factors on the electrostacking pre-concentration, as well as the electric field strength and ionic mobility. The method developed was suitable for the simultaneous separatio…
Green direct determination of mineral elements in artichokes by infrared spectroscopy and X-ray fluorescence.
Near infrared (NIR) and X-ray fluorescence (XRF) spectroscopy were investigated to predict the concentration of calcium, potassium, iron, magnesium, manganese and zinc in artichoke samples. Sixty artichokes were purchased from different Spanish areas (Benicarlo, Valencia and Murcia). NIR and XRF spectra, combined with partial least squares (PLS) data treatment, were used to develop chemometric models for the prediction of mineral concentration. To obtain reference data, samples were mineralised and analysed by inductively coupled plasma optical emission spectrometry (ICP-OES). Coefficients of determination obtained for the regression between predicted values and reference ones for calcium, …
Removal of Hexavalent Chromium from Aqueous Solutions Using Biopolymers
AbstractTwo biopolymers were prepared by reaction of chestnut and quebracho tannins with gelatin extracted from untanned hide wastes. Obtained biopolymers were evaluated as adsorbents for removing ...
ICP-MS multielement determination in fly ash after microwave-assisted digestion of samples.
A microwave assisted digestion procedure has been developed for dissolution of fly ash samples prior to the inductively coupled plasma-mass spectrometric determination of their elemental composition. The developed methodology was validated by carrying out the analysis of two high-silicate containing reference materials (CRM 134R sewage amended soil and NIES JR 1 rock) and by means of the comparison between results found by microwave-assisted digestion and ICP-MS of fly ash samples with those found by neutron activation analysis (NAA) for Sb, Cs, Cr, Co, Fe, U and Zn determination. The method developed can be recommended for routine multielement analysis of fly ash.
Determination of ultratrace bismuth in milk samples by atomic fluorescence spectrometry.
Abstract A sensitive procedure was developed for determination of bismuth (Bi) in milk samples by hydride generation atomic fluorescence spectrometry (HG–AFS) after microwave-assisted sample digestion with HNO3 and H2O2. The method provides a sensitivity of 1832 fluorescence units (ng/mL) with a detection limit of 0.01 ng/mL, which corresponds to 20 pg absolute limit of detection, equivalent to 0.50 ng/g in the original sample. Application of the methodology to cow milk samples from the Spanish market showed the presence of Bi at a concentration of 11.8–28.8 ng/g, which compared well with data obtained after dry ashing of samples and with data obtained by inductively coupled plasma–mass spe…
Determination of mercury in rice by cold vapor atomic fluorescence spectrometry after microwave-assisted digestion.
Abstract A cold vapor atomic fluorescence spectrometry method (CV-AFS) has been developed for the determination of Hg in rice samples at a few ng g−1 concentration level. The method is based on the previous digestion of samples in a microwave oven with HNO3 and H2O2 followed by dilution with water containing KBr/KBrO3 and hydroxylamine and reduction with SnCl2 in HCl using external calibration. The matrix interferences and the effect of nitrogen oxide vapors have been evaluated and the method validated using a certified reference material. The limit of detection of the method was 0.9 ng g−1 with a recovery percentage of 95 ± 4% at an added concentration of 5 ng g−1. The concentration level …