Determination of gallium in tumour-affected tissues by means of spectroscopic techniques

A comparative investigation was carried out on the suitability of atomic absorption spectrometry and of emission spectrography with arc and hollow-cathode excitation sources for determination of gallium (μg g^-1) in biological samples. The three methods give reliable results. Hollow-cathode emission spectrography was found to be influenced to a lesser extent by matrix effects and to be more precise than the other two techniques.     

Discovering the composition of ancient cosmetics and remedies: analytical techniques and materials

This article reviews the analytical techniques and procedures used in the study of ancient cosmetics, therapeutic chemicals, and remedies found in historical and archaeological sites. Well consolidated techniques based on molecular and atomic spectroscopy, for example FT-IR, Raman, SEM-EDX, and XRD, and analytical procedures based on high-performance chromatography and mass spectrometry, for example GC–MS and HPLC–MS are reviewed. The advantages of recently introduced techniques based on synchrotron radiation and on direct mass spectrometric techniques are also discussed. The possibility of extracting information about composition, preparation techniques, and the degradation processes of ancient cosmetics, pharmaceutics, and ritual balms is analysed by use of several case studies.     

A crystallinity study of dental tissues and tartar by infrared spectroscopy

In this paper we report a study of an important property of biomineralized phases, crystallinity, on the basis of previous results for synthetic apatite. Crystallinity is not only important for understanding biomineralization, it is also related to the maturation and mechanisms of growth of calcium phosphates in biological surroundings. We studied two kinds of sample, teeth as an example of biomineralized tissues and dental calculi (adhering) as an example of mineralization without participation of biological agents, except possibly bacteria. The investigation focused on study of ν(1)-ν(3) infrared absorption bands of PO(4)(3-) phosphates. We used ATR (attenuated total reflection) analysis to examine human dental tissues and tartar on several samples. The results confirm for the first time previous assumptions about the growth and maturation of dental calculi, i.e., crystallinity progresses from regions of high crystallinity to regions of lower crystallinity, and, in addition, its quantification with spatial resolution in the sample. A gradual pattern was observed in dental calculus. Another result from this study was that cementum and dentine had similar crystallinity, despite their different biological and mechanical functions.     

Elemental composition of seasoning products

The elemental composition of seasoning products, like spices garlic and onion, has been reviewed paying special attention to methods proposed in the literature to determine specific elements or as much as possible components of these products which are widespread used in food preservation or food flavouring and can contribute to the intake of both, essential and toxic elements. Sample treatment and metal speciation aspects have been critically revised concerning onion, garlic and pepper (the most commonly studied products).     

Comparability of data for natural radionuclides in marine sediment obtained by different analytical techniques

In the paper are presented results of potassium, uranium, thorium and radium measurements performed on the natural marine sediment sample SD-N-1/2 in the framework of the IAEA-organized worldwide intercomparison exercise. Analytical methods applied in this exercise were evaluated for performance and significance of the observed discrepancies are discussed in the light of statistical and operative criteria. Possible sources of error have been identified in alpha and gamma spectrometric measurements and suggestions are given about how to avoid them. Well characterized reference materials based on natural matrices have been shown helpful in achieving better data comparability in low level measurements of environmental radioactivity.     

The study of stabilizer action modes by means of time-resolved techniques: Intermediate radical cations

In organic systems, radiation- and photo-induced electron transfer reactions result in the first step in the formation of radical cations. With pulse radiolysis and laser photolysis experiments radical cations of phenols could be indirectly characterized whereas radical cations of sterically hindered amines (HALS compounds) could be directly observed.     

Reliable screening of various foodstuffs with respect to their irradiation status: A comparative study of different analytical techniques

Cost-effective and time-efficient analytical techniques are required to screen large food lots in accordance to their irradiation status. Gamma-irradiated (0–10 kGy) cinnamon, red pepper, black pepper, and fresh paprika were investigated using photostimulated luminescence (PSL), direct epifluorescent filter technique/the aerobic plate count (DEFT/APC), and electronic-nose (e-nose) analyses. The screening results were also confirmed with thermoluminescence analysis. PSL analysis discriminated between irradiated (positive, >5000 PCs) and non-irradiated (negative, <700 PCs) cinnamon and red peppers. Black pepper had intermediate results (700–5000 PCs), while paprika had low sensitivity (negative results) upon irradiation. The DEFT/APC technique also showed clear screening results through the changes in microbial profiles, where the best results were found in paprika, followed by red pepper and cinnamon. E-nose analysis showed a dose-dependent discrimination in volatile profiles upon irradiation through principal component analysis. These methods can be used considering their potential applications for the screening analysis of irradiated foods.     

Moss as monitor of heavy metal deposition: Comparison of different multi-element analytical techniques

Instrumental activation analysis (INAA) based on irradiations in a nuclear reactor with particularly high relative fluxes of resonance and fast neutrons has been shown to open new possibilities for multi-element surveys of mosses used as monitors of atmospheric deposition. Comparison is made with data obtained by inductively coupled plasma-mass spectrometry (ICP-MS) and conventional INAA. Data for 15 elements not previously investigated in routine moss studies are presented, e.g., Zr, Sn, Hf, Ta, W, Au, Th, and the rare earth elements Ce, Nd, Eu, Gd, Tb, Tm, Yb, Lu. Other elements particularly well determined by this approach are Sc, Co, As, Ag, Sb, Cs, La, Sm, Th, and the non-metallic trace elements Se, Br, and I. Advantages and drawbacks with the high fast neutron component are discussed.     

Investigation of different types of filters for atmospheric trace elements analysis by three analytical techniques

Different atmospheric aerosol samples were collected on three types of filters. Disks of both loaded and clean areas of each kind of filter were investigated by XRF, PIXE and Scanning Electron Microscope (SEM) methods. The blank concentration values of the elements Al, Si, P, S, Cl, K, Ca, Sc, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, As, Br and Pb in the three types of fiters are discussed. It is found that for trace elemental analysis, the Nuclepore membrane filters are the most suitable for sampling. These have much lower blank element concentration values than the glass fibres and ash free filters. It was found also that the PIXE method is a more reliable analytical technique for atmospheric aerosol particles than the other methods.     

Review of the applications of different analytical techniques for coxibs research

An extensive survey of the literature published in analytical and pharmaceutical chemistry journals has been conducted and analytical methods which were developed and used for the determination of some of the COX-2 inhibitors, a subclass of non-steroidal anti-inflammatory drugs (NSAIDs) in bulk drugs, formulations, and biological fluids have been reviewed. This review covers the time period from 1999 to present, during which over 140 analytical procedures including chromatographic, spectrometric, electrophoretic and voltammetric techniques were reported. Presented applications concern analysis of coxibs from pharmaceutical formulations and biological samples.     

Elemental composition of organic and non-organic foods determined by PIXE

Journal of Radioanalytical and Nuclear Chemistry - Nutrition and safety of foods is one of the more discussed topics in the modern society. We processed twenty food samples of the organic and...     

Elemental composition of skin tissue by PIXE and INA analyses

Hypertrophic scars are a particular type of scar that can form after any type of dermal injury. They are unsightly, red, elevated above nomal skin level, itchy and painful. At present no-one knows why these scars form. Due to the differences between scar tissue and normal skin it was decided to analyse skin tissue which at a later date would be compared to scar tissue. Split skin graft (epidemis) samples as well as full thickness skin (epidemis to demis) tissue were analysed using PIXE and RBS with a 2 MeV proton beam. The epidemis was compared to the demis to see if there were any variations between the two. In all the samples P, S, Cl, K, Ca, Fe, and Cd were detected and in a majority of the samples Zn and Ba were found, using PIXE. It was found that, between the epidemis and demis, there was an significant increase in P in the epidermis in both full thickness and split skin graft samples. Complementary elemental analysis was also performed using neutron activation, and Br, Na and Zn were detected.     

Elemental composition of Nigerian harmattan dust

Six samples of harmattan dust collected over three seasons of harmattan in Nigeria were analyzed for 29 elements by instrumental neutron activation analysis. The mean concentrations are (in g/g): Al, 61100; As, 6.59; Au, 0.16; Ba, 695; Br, 195; Ce, 122; Cl, 6200; Co, 20.9; Cr, 119; Cs, 2.72; Eu, 1.31; Fe, 43 1000; Ga, 21.9; Hf, 8.05; K, 15700; La, 53.9; Mg, 8700; Mn, 825; Na, 6400; Rb, 82.4; Sb, 32.7; Sc, 10.3; Se, 6.61; Sm, 6.50; Th, 14.0; Ti, 4900; U, 6.28; V, 81.6; Zn, 2200. The results are compared to similar recent studies in the German Democratic Republic.     

Elemental composition of air masses under different altitudes in Azores,central north Atlantic

Between 8th July 2002 and 18th June 2004, aerosol samples were collected in Azores. Their inorganic composition was obtained by neutron activation analysis in order to study the differences of aerosols in two atmospheric altitudes of the central north Atlantic: (1) PICO-NARE observatory (Lower Free Troposphere-LFT) at Pico mountain summit (38,470oN, 28,404oW, 2,225 m a.s.l.) in Pico Island, Azores, where air masses from the surrounding continents (Africa, Europe, Central and North America) pass through, carrying aerosols with anthropogenic (Sb, Br, Mo, U, Se and Tb) and/or natural emissions (Fe, Co, La, Na, Sm, Cr, Zn, Hf, K and Th); (2) TERCEIRA-NARE station (Marine Boundary Layer) at Serreta (38,69oN, 27,36oW, 50 m a.s.l.), in Terceira Island, Azores, where natural aerosols (I, Cl, Na, Br and other soil related elements) are predominant. However, a combined interpretation of the data points out to a co-existence of the anthropogenic elements Sb and Mo, eventually with similar origins as the ones passing Pico Mountain summit. Very high concentrations and enrichment factors for Sb, Mo and Br in LFT, higher than the ones found in other areas, confirm atmospheric long-range transport mainly from the west boundary of north Atlantic; this may indicate eventual accumulation and persistence of those elements in the area due to the presence of Azores high pressures or the Hadley cells effect. A significant correlation between Fe and Yb and the enrichment of rare earth elements (La, Sm, Tb and Yb) and Th in LFT aerosols, both reflect a mineral dust intrusions from north Africa (Sahara and Sahel region).     

Elemental composition changes in citrus affected by the CVC disease

The citrus variegated chlorosis (CVC) disease results in serious economical losses for the Brazilian citriculture. The influence of CVC disease on the elemental composition of citrus plants was investigated. Leaves of sweet orange varieties Hamlin, Pera Rio and Valencia were collected from healthy and CVC-affected trees for chemical characterization by instrumental neutron activation analysis (INAA). Significant differences between healthy and CVC-affected leaves were identified for Ca, Ce, Co, Eu, Fe, K, La, Na, Nd, Rb, Sc and Sm. Rare earth elements presented consistently higher mass fractions in the healthy leaves.     

Integrated analytical techniques for the study of ancient Greek polychromy

The materials used in the decoration of three painted astragaloi (knucklebones) from the Koroneia cave (Greece) were investigated by means of sequential application of non-destructive and destructive techniques: optical microscopy, environmental scanning electron microscopy coupled with X-ray microanalysis (ESEM-EDX), Fourier transform infrared spectroscopy (FTIR) with micro-attenuated total reflection (μ-ATR) technique, high performance liquid chromatography (HPLC) coupled with UV-fluorescence and gas chromatography-mass spectrometry (GC-MS) were used.The main results highlighted that the three astragaloi were prepared with a ground of ochre or iron clay and painted with a proteinaceous matter such as binder egg tempera. Both FTIR and GC-MS agree in the detection of lipids that can be related to egg. Organic dyestuffs identified as madder lake and shellfish purple were used together with inorganic pigments.     

Study of 32P in n-irradiated ammonium hypophosphite using different analytical techniques

³²P in n-irradiated ammonium hypophosphite has been studied by three different analytical techniques; classical aqueous, non-aqueous and thin layer chromatographic analysis, the latter using a non-aqueous solvent. A comparison of the results obtained by the three methods shows that (a) P(V) valence state is a hydrolytic product, (b) P(III) valence state arises from an independent precursor in the solid state and (c) there are at least three precursors for the P(I) valence state.     

The diethyldithiocarbamate of mercury: composition,structure and analytical application: A heterometric study

0.3–1.2 mg of mercury (= Hg(NO₃)₂) in 20 ml aqueous solution, can be titrated heterometrically with sodium diethyldithiocarbamate (NaCBM).Vice versa, 0.5–1.0 mg NaCBM in 20 ml aqueous solution can be titrated heterometrically with mercuric nitrate.In both cases the error is mostly equal to zero. The insoluble Hg(CBM)₂ is obtained in both cases.