Estimation of trace elements in some anti-epileptic medicinal plants by PIXE

Trace elemental analysis was carried out in various parts of 10 anti-epileptic medicinal plants using PIXE technique. A 3?MeV proton beam was used to excite the samples and spectra were recorded using a Si(Li) detector. Data analysis was done using Gupix Software. The elements Cl, K, Ca, Ti, Mn, Fe, Ni, Cu, Zn, Br and Sr were identified and their concentrations estimated. The presence of some of these trace elements is correlated with the anti-epileptic curative property of these plants.     

Quantitative multielemental analysis of titaniferous magnetites

Two representative titaniferous magnetite samples procured from Moulabhanj, Orissa, India have been studied by PIXE, EDXRF, Mössbauer spectroscopy, and XRD techniques. Major iron-bearing phases identified in the samples by Mössbauer spectroscopy and XRD are magnetite, hematite, ferrous ilmenite and ferric ilmenite. The Fe²⁺/Fe³⁺ ratio and the relative percentages of different minerals were determined from the resonance areas of Mössbauer spectra. Quantitative multielemental analysis was carried out by energy dispersive X-ray fluorescence (EDXRF) and proton induced X-ray emission (PIXE). Nineteen minor and trace elements have been quantified by EDXRF whereas by PIXE eighteen elements have been analyzed quantitatively. Concentrations of trace elements determined by EDXRF and PIXE were used in interpreting the physico-chemical condition of the depositional basin.     

Use of different spectroscopic techniques in the analysis of Roman age wall paintings

In this paper the analysis of samples of Roman age wall paintings coming from: Pordenone, Vicenza and Verona is carried out by using three different techniques: energy dispersive x-rays spectroscopy (EDS), x-rays fluorescence (XRF) and proton induced x-rays emission (PIXE). The features of the three spectroscopic techniques in the analysis of samples of archaeological interest are discussed. The studied pigments were: cinnabar, yellow ochre, green earth, Egyptian blue and carbon black.     

External proton beam analysis of layered objects

Ion-beam analysis for determining the elemental composition and to obtain depth information has been carried out with MeV protons in air by means of simultaneous external PIXE and RBS. Stainless steel products of extended size and a historic painting are analyzed non-destructively. These objects include systems of layers with areal densities up to some ten mg/cm². Depth information is obtained by PIXE using energy variation of the primary proton beam and in addition directly from RBS for the outermost near-surface region. Main and secondary elements as well as impurities can be determined together with areal densities. Particularly, the knowledge on the depth distribution of the pigments in paintings provides information on paint techniques.     

Multitechnique characterization of lapis lazuli for provenance study

Lapis lazuli is one of the oldest precious stone, being used for glyptic as early as 7,000 years ago: jewels, amulets, seals, and inlays are examples of objects produced using this material. Only a few sources of lapis lazuli exist in the world due to the low probability of geological conditions in which it can form, so that the possibility to associate the raw material to man-made objects helps to reconstruct trade routes. Since art objects produced using lapis lazuli are valuable, only nondestructive investigations can be carried out to identify the provenance of the raw materials. Ionoluminescence (IL) is a good candidate for this task. Similar to cathodoluminescence (CL), IL consists in the collection of luminescence spectra induced by megaelectronvolt ion (usually protons) irradiation. The main advantage of IL consists in the possibility of working in air while measuring simultaneously the composition of major and trace elements by means of complementary ion beam analysis techniques like particle-induced X-ray emission (PIXE) or particle-induced gamma-ray emission (PIGE). In the present work, a systematic study of the luminescence properties of lapis lazuli under charged particle irradiation is reported. In the first phase, a multitechnique approach was adopted (CL, scanning electron microscopy with microanalysis, micro-Raman) to characterize luminescent minerals. This characterization was propaedeutic for IL/PIXE/PIGE measurements carried out on significant areas selected on the basis of results obtained previously. Criteria to identify provenance of lapis lazuli from four of the main sources (Afghanistan, Pamir Mountains in Tajikistan, Chile, and Siberia) were proposed.     

The analysis of air particulate deposits using 2 MeV protons

Particle-induced X-ray emission (PIXE) analysis of the lighter elements in time-resolved air particulate deposits has been carried out. Minimum detection limits have been determined for 1.0, 2.0 and 3.5 MeVprotons. Quantitative PIXE analysis results, obtained with 2 MeV protons, are given for temporal variations in the elemental concentrations of Na, Al, Si, S, Cl, K, Ca and Fe. Rutherford backscattering (RBS) spectra were taken simultaneously with the PIXE spectra to provide information on lead concentrations and deposit thicknesses. The experimental problems associated with the quantitative analysis of light elements on cellulose acetate filters are described. The relationship between these results and meteorological data is discussed.     

External proton beam analysis of layered objects

Ion-beam analysis for determining the elemental composition and to obtain depth information has been carried out with MeV protons in air by means of simultaneous external PIXE and RBS. Stainless steel products of extended size and a historic painting are analyzed non-destructively. These objects include systems of layers with areal densities up to some ten mg/cm(2). Depth information is obtained by PIXE using energy variation of the primary proton beam and in addition directly from RBS for the outermost near-surface region. Main and secondary elements as well as impurities can be determined together with areal densities. Particularly, the knowledge on the depth distribution of the pigments in paintings provides information on paint techniques.     

Sulfur-Doped n-Type Diamond: Preparation and Electrochemical Properties

Films of sulfur-doped synthetic diamond are chemical-vapor-deposited using codoping with sulfur and boron. The sulfur in diamond is detected with particle-induced x-ray emission (PIXE), x-ray photoelectron spectroscopy (XPS), and secondary ion mass spectroscopy (SIMS). Electrochemical and thermoelectric measurements show that the sulfur-containing diamond films grown in gas phase lean in boron are n-type, whereas those grown with higher boron content are overcompensated, hence, p-type. Electrochemical properties of the n-type diamond films are studied for the first time using methods of electrochemical impedance, open-circuit photopotential, and voltammetric curves in Fe(CN)₆ ^3-/4- solutions. A mechanism of boron-stimulated sulfur incorporation into diamond and the nature of donors thus formed is discussed.     

Standardless PIXE analysis of thick biomineral structures

The particle-induced X-ray emission (PIXE) of thick biomineral targets provides pertinent surface analysis, but if good reference materials are missing then complementary approaches are required to handle the matrix effects. This is illustrated by our results from qualitative and semiquantitative analysis of biomaterials and calcified tissues in which PIXE usually detected up to 20 elements with Z > 14 per sample, many at trace levels. Relative concentrations allow the classification of dental composites according to the mean Z and by multivariate statistics. In femur bones from streptozotocin-induced diabetic rats, trace element changes showed high individual variability but correlated to each other, and multivariate statistics improved discrimination of abnormal pathology. Changes on the in vitro demineralization of dental enamel suggested that a dissolution of Ca compounds in the outermost layer results in the uncovering of deeper layers containing higher trace element levels. Thus, in spite of significant limitations, standardless PIXE analysis of thick biomineral samples together with proper additional procedures can provide relevant information in biomedical research.Abbreviations AAS Atomic absorption spectrometry - ERDA Elastic recoil detection analysis - ESR Electron spin resonance - FDA Factorial discriminant analysis - FTIR spectroscopy Fourier transform infra-red spectroscopy - HP Ge detector Hyperpure Ge detector - ICP-AES Inductively coupled plasma atomic emission spectrometry - NAA Neutron activation analysis - NRA Nuclear reaction analysis - PCA Principal component analysis - PIXE Particle-induced X-ray emission - PIGE Particle-induced -ray emission - RBS Rutherford backscattering spectroscopy - SRIXE Synchrotron radiation-induced X-ray emission     

Trace Metals in Microcrustaceans and Brazilian Waterweed from a Contaminated Chilean Wetland Using Total Reflection X-Ray Fluorescence Spectrometry

The trace element content of individual copepod specimens and of the Brazilian water weed (Egeria densa) from a metal-contaminated wetland in Southern Chile were determined using total reflection X-ray fluorescence spectrometry. Sampling of the water and the organisms was carried out at three sampling sites during 2004. Enhanced concentrations of dissolved Fe and Mn were found in the column water and in the pore water. The Fe content in the benthic copepods was significantly elevated compared to other aquatic organisms from different Chilean lakes. Regarding E. densa, healthy (green coloured) plants showed mass fractions of Fe, Mn, Ni, Cu and Zn which were typical for uncontaminated systems. In contrast, damaged (brownish coloured) plants exhibited very high Fe and Mn concentrations indicative of contamination or processes which changed the element load from the environment to the plant.     

Determination of chemical elements in airborne particulate matter collected at Lembang, Indonesia by particle induced X-ray emission

Monitoring the air quality in ambient air is an important step for assessing the air pollution level in one region and its impact to the human health. In this study, the determination of chemical elements concentrations in airborne particulate matter collected in suburban area of Lembang, Indonesia was carried out. Samples were collected using a Gent stacked filter unit sampler in two size fractions of <2.5 μm (fine) and 2.5–10 μm (coarse). Sampling was conducted twice a week for 24 h from January 2008 to June 2009 and 123 pairs of samples were collected. Black carbon was determined by reflectance and chemical elements analysis were performed using particle induced X-ray emission (PIXE). PIXE as one of ion beam analysis techniques is suitable for analyzing particulate matter for its multielemental analysis with good limits of detection. Results showed that none of daily concentrations of PM_2.5 and PM₁₀ exceeded the 24 h Indonesian NAAQS for PM_2.5 and PM₁₀. Chemical elements such as Mg, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, As, Hg and Pb were determined and the correlation between these elements was reported in order to understand the anthropogenic sources of particulate matter.     

Combined application of INAA and PIXE for studying the regional aerosol composition in Southern Africa

As part of the SAFARI-92 biomass buming experiment, aerosol collections were carried out with several size-fractionating sampling devices at a number of sites in Southern Africa. One of the samplers used at all ground-based sites was a stacked filter unit (SFU). The SFU samples were analyzed by both INAA and PIXE analysis. The present paper gives an intercomparison of the analytical results obtained in order to assess the accuracy and to check the quality assurance of the analytical procedures. Twenty-one common elements were determined by both INAA and PIXE. Concentrations of 13 elements (i.e., Na, Mg, Al, Cl, K, Ca, Ti, V, Cr, Mn, Fe, Zn and Br) were generally measured with sufficient precision in both techniques for performing the intercomparison. The INAA and PIXE data were compared in terms of PIXE/INAA concentration ratios on a sample by sample basis for the coarse and fine size fraction separately. the atmospheric concentrations for K, Mn and Fe agreed within 5–10%, the agreement between the data for the other common elements was typically better than 15%. Possible explanations for lower than 1.0 ratios for Cl, Br and Na are presented. The common elements were classified into groups according to their detectability and sensitivity in each technique.     

Particle Induced X-Ray Emission (PIXE) Analysis of Basella Alba L Leaves

Six groups of Basella Alba L plants grown in different conditions were analysed by using particle induced X-ray emission (PIXE) method to establish a relationship between the elemental map and growth fertiliser conditions. The target samples were bombarded with a 3 MeV protons beam at the tandem accelerator of IFIN-HH Bucharest and the X-rays were detected with a HPGe detector with a 160 eV resolution at the 6.4 keV of K line of iron. The concentrations obtained have an estimated error of less then 6% for most of the elements analysed.     

Facile extraction of berberine from different plants,separation, and identification by thin-layer chromatography,high-performance liquid chromatography,and biological evaluation against Leishmaniosis

The extraction of berberine was carried out from Berberis vulgaris, Berberis aquifolium, and Hydrastis canadensis plants using ethanol and water (70:30, v/v). The extracted berberine was characterized by ultraviolet-visible and Fourier-transform infrared spectroscopy. The purity of berberine was ascertained by thin-layer chromatography using n-propanol-formic acid-water (95:1:4) and (90:1:9) solvents. hR_f values were in the range of 44–49 with compact spots (diameter 0.2–0.4 cm). HPLC was carried out using ammonium acetate buffer and acetonitrile in gradient mode with Zodiac (4.6 × 150 mm, 3 μm) column. The flow rate was 1.0 mL/min and detection was at 220 nm. The values of separation and resolution factors of the standard and the extracted berberine were in the range of 1.13–1.16 and 1.40–1.71, respectively. A comparison has shown that both thin-layer chromatography and high-performance liquid chromatography (HPLC) methods found applications in different situations and requirements. The extracted berberine samples were used to treat Leishmaniosis and the results showed better activity of berberine in comparison to the standard drug Amphotericin B. Briefly, the reported research is a novel and may be used to extract berberine from plants, separation and identification of berberine by thin layer chromatography and HPLC and to treat Leishmaniosis.     

Determination of aluminium and silicon in zeolites by PIXE

Using 1.0 MeV protons on thick targets of zeolite pellets, aluminium and silicon were determined by PIXE. Results were compared with XRF data. The relative root mean square error was 3.7% and the results of the two methods agreed with a correlation factor of 0.991. PIXE analysis can be carried out on very small samples, while sample preparation involves minimal handling.     

The use of vetiver for remediation of heavy metal soil contamination

The use of Vetiveria zizanioides (vetiver) was studied to evaluate its efficiency for the remediation of soils contaminated by heavy metals. Vetiver plants were tested for Cr, Cu, Pb and Zn. Phytoextraction and bioremediation experiments were carried out by irrigating the vetiver plants and the dry plants with solutions containing suitable amounts of Cr, Cu, Pd and Zn. The concentrations of the heavy metals were determined in both experiments in shoot and root parts of vetiver plants using inductively coupled plasma atomic emission spectroscopy after a mineralization step. Phytoextraction experiments showed a poor efficiency of vetiver for Cr and Cu uptake (both less than 0.1% in shoots and roots after 30 days), but a quite high capability of Pb and Zn uptake (0.4% in shoots and 1% in roots for Pb and 1% both in shoots and in roots for Zn, after 30 days). For these reasons the vetiver plant can be considered a quite good “hyperaccumulator” only for Pb and Zn. As for bioremediation experiments, the vetiver plant showed heavy metal uptake values significantly lower than those obtained with other biological substrates. Figure Vetiver plant     

In Vitro Plant Propagation of Catharanthus roseus and Assessment of Genetic Fidelity of Micropropagated Plants by RAPD Marker Assay

An investigation was carried out to develop an efficient micropropagation protocol for Catharanthus roseus. Experiments were conducted to optimize suitable media for in vitro shoot multiplication and root induction. Out of the different media compared for in vitro shoot multiplication, Murashige and Skoog (MS) medium supplemented with 1 mg/l of 6-benzylaminopurine and 0.2 mg/l α-naphthaleneacetic acid showed better response in terms of the emergence of shoots from axillary buds as well as proliferation and multiplication of shoots. The shoots when placed on half strength of MS medium having 1 mg/l indole 3-butyric acid and 0.25 % charcoal showed cent percent root induction with maximum number of roots per shoot (4.2) as well as maximum root length (1.72 cm). Further, clonal fidelity of the in vitro-raised plants was carried out using randomly amplified polymorphic DNA marker and results indicated that all the tissue culture-derived plants are true-to-type and there were no somaclonal variations among these plants.     

Study on the retention of uranyl ions on modified clays with titanium oxide

Four analytical techniques—instrumental neutron activation analysis (INAA), inductively coupled plasma mass spectrometry (ICP-MS), scanning electron microscope energy dispersive X-ray fluorescence (SEM-EDXRF), and proton induced X-ray emission (PIXE)—were evaluated in the context of air pollution biomonitoring studies. Three combinations INAA/ICP-MS, ICP-MS/PIXE and ICP-MS/SEM-EDXRF are illustrated by experimental results.     

Absolute structure determination using CRYSTALS

A study of post‐refinement absolute structure determination using previously published data was carried out using the CRYSTALS software package. We show that absolute structure determination may be carried out optimally using the analyses available in CRYSTALS, and that it is not necessary to have the separate procedures absolute structure determination and no interest in absolute structure as proposed by Flack [Chimia (2014), 68 , 26–30].