Elemental analysis of limestone by instrumental neutron activation analysis

Limestone samples from Assuit Governrate in Upper Egypt were subjected to elemental analysis by instrumental neutron activation analysis and X-ray fluorescence techniques. The samples were properly prepared together with their standards and simultaneously irradiated in a neutron flux of the order 7 × 1011 n/cm² s using TRIGA research reactor at Mainz. After activation the samples were subjected to γ-ray spectrometry using a high purity germanium detection system and computerized multichannel analyzer. Nineteen elements: Na, Ca, Mn, Fe, Sc, Cr, Co, Zn, Sn, La, Ce, Nd, Eu, Sm, Yb, Lu, Hf, Th and U were analyzed. X-ray fluorescence spectrometry have been also used. The presence of any elements in higher or lower levels in certain limestone samples is contingent on the occurrence of its bearing minerals, nature of parent sediments and depositional environments of these sediments. The major elements in the samples were also observed to be among the elements that had high enrichment factors in the study of suspended dust particulate within and around cement industries. This confirms cement as the major contributor to the airborne particulate matter in the environs.     

Elemental analysis of soils from Toshki by using instrumental neutron activation analysis techniques

Instrumental neutron activation analysis has allowed performing a complete characterization of the chemical composition of thirty soil samples soil samples from ten locations collected from the Toshki area in Upper Egypt. The samples were irradiated with thermal neutrons at the Mainz TRIGA research reactor. Gamma-ray spectra were recorded using a high efficiency HPGe detector to determine the contents of major, minor and trace elements in these samples. As a result of the analysis, altogether 32 elements were identified qualitatively and quantitatively. These elements are: Al, As, Ba, Ca, Ce, Co, Cr, Cs, Eu, Fe, Ga, Hf, K, La, Lu, Mg, Mn, Na, Nb, Nd, Rb, Sc, Sm, Sn, Ta, Ti, Th, U, V, Yb, Zn and Zr. In several cases, X-ray fluorescence analysis was used for comparison. The results obtained for U and Th were compared with data reported in literature.     

Trace-element analysis of argyle diamonds using instrumental neutron activation analysis

Thirty four elements were determined by instrumental neutron activation analysis in colourless, brown, and pink diamonds, with and without inclusions. These were compared with data obtained for similar elements in the host lamproite rock. The natural radioactivity of these samples was measured by instrumental techniques, and found to be negligible.     

A provenance study of coffee by photon activation analysis

Photon activation analysis (PAA) is a multi-elemental radioanalytical technique in trace elements analysis with high accuracy and precision. Researchers at the Idaho accelerator center performed PAA analysis on coffee samples from several locations around the world as an initial step in assessing the relationship between trace elements in illicit drugs and the soils in which they were grown. The preliminary results show coffees from different locations have different concentrations of trace elements. In the three cases where we have soil samples, the matrices of elements in the coffee samples are closely related to the matrices of the elements of the local soil samples. The majority of trace elemental content is similar to that of the local soil sample in which the coffee is planted. It may be that coffee assimilates numerous elements from the soil where it is grown in similar ratios as is found in the soil. Thus, it is conceivable that the elemental content could serve as “fingerprint” to trace the origins of the coffee. To verify our analytical results we applied X-ray fluorescence (XRF) methods as well. Our PAA results are consistent with XRF experimental data. The future of tracing the origin of illicit drugs with the PAA technique is promising.     

Atmospheric deposition of heavy metals in Norway studied by the analysis of moss samples using neutron activation analysis and atomic absorption spectrometry

In a study of the atmospheric deposition of trace elements in different parts of Norway, samples of the mossHylocomium Splendens were analyzed with respect to 28 elements. The determination of Cu, Zn, Cd, and Pb was carried out by atomic absorption spectrophotometry, while 24 additional elements were determined by instrumental neutron activation analysis. In samples from southernmost Norway, a substantially higher concentration was found for elements such as Pb, Sb, V, Cr, Cu, Zn, As, Se, Mo, Ag, and Cd than in samples from places located in the more northerly parts of the country. The results indicate that sources which are to the south and south-west of Scandinavia, contribute significantly to heavy metal deposition in Norway.     

Elemental analysis of traditional medicinal seeds by instrumental neutron activation analysis

Traditional medicinal seeds prescribed for specific treatment purposes, were purchased from local markets and analyzed by INAA. The samples were irradiated at Es-Salam research reactor, at a power of 5 MW for 6 h. The accuracy of the method was established by analyzing reference materials. Twenty elements were measured, with good accuracy and reproducibility. The concentration of elements determined, was found to vary depending on the seeds. The daily intake of essential and toxic elements was determined, and compared with the recommended values. The probable cumulative intake of toxic elements is well below the tolerance limits.     

Multielement trace analysis of high purity aluminium by neutron activation

Instrumental neutron activation analysis was applied to multielement trace analysis of high purity aluminium samples. In order to reduce the production of²⁴Na from the matrix, samples were activated by thermal neutron flux of high cadmium ratio. Detection limits of various impurity elements were evaluated. So called “five nine” class standard aluminium samples were analyzed and concentrations of various impurity elements were determined. The analytical results obtained on zone refined aluminium samples showed that zone refining is effective against many elements, such as Na, Cr, Fe, Co, Cu, Ga, As, Br, Ba, La, Ce, Sm, Yb, Lu, Hf, W, Th and U, but not very effective against the element Sc.     

Geostandards and geochemical analysis

Progress in geochemical analysis depends on progress in geostandards. The present state of the availability and quality of the geostandards is reviewed for major and trace elements. The several geochemical methods employed are evaluated by their performances in the characterization of geostandards. Signs of progress are visible in the quality of geostandards for major and “common” trace elements. There are also new developments in geoanalytical methods. It is hoped that optical emission inductively coupled plasma spectrometry will play an increasing role in the characterization of trace elements which are normally present in less than 10 ppm concentration levels.Like it or not, progress in geochemical analysis is intimately tied up with the quality of geochemical reference samples (GRS). The converse is true as well; therefore, how well and to what extent international geochemical reference samples are characterized for their chemical composition reflect in a way the current status of geoanalytical methods employed the world over.     

Determination of the chemical composition of the South Pole aerosol by instrumental neutron activation analysis

Atmospheric particulate samples were collected at the geographic South pole, using cellulose and polycarbonate filters and cascade impactors. The samples were analysed for 40 elements by instrumental neutron activation analysis. From the filter samples atmospheric concentrations for 33 elements could be obtained. The highest atmospheric concentrations were found for S: 49 ng/standard cubic meter (SCM) of air, Na: 3.3 ng/SCM and Cl: 2.6 ng/SCM. In the cascade impactor samples, only a few elements were observed above blank. For these elements it could be concluded that they are associated for over 80–90% with submicron size paricles.     

Neutron activation analysis of indium

The extraction and extraction-chromatographic behavior of many elements in the tributylphosphate — HBr solution system has been studied. The investigation performed has made it possible to develop a simple technique for neutron activation determination of 22 impurity elements in high purity indium samples with detection limits from 0.1 ppm for Fe and Zr to 0.01 ppb for Na, Sc, Cu, As, La and W.     

Instrumental thermal neutron activation analysis of tobacco

A group of 27 tobacco samples was submitted to INAA. Bowen's Kale was analyzed with the samples. The resulting data for 21 elements in tobacco were processed by a cluster programme. This combination proves to be a convenient tool for discrimination within one group of samples.     

Pattern recognition analysis for characterization of coal and ash samples

Different pattern recognition techniques were applied for classification and characterization of a large number of coal, and coal fly ash samples. Cluster analysis was performed on 116 samples using the concentration data of 40 elements. The effect of the number and type of the elements on the clustering was studied in detail. It was proved that short time activation analysis enables the characterization of these types of samples if¹³⁹Ba and⁸⁷Sr are included, these data being obtained by increasing the irradiation and counting times. The two elements and chlorine were found to be necessary for such a classification. The combination between cluster analyses and principal component analysis gives accurate and confirmed results. The statistical analyses of the subgroups are compared.     

Characterization of Costa Rican potsherds by neutron activation analysis

Neutron activation analysis has been applied to evaluate the concentrations of 24 elements in archaeological potsherds and 5 clay samples with a view of establishing the average composition profiles. Due to their stability in clays, 14 elements were selected as indicators. A statistical treatment of the overall analytical data, including principal component analysis, was applied in an attempt to determine correlations between the concentrations of the elements in the samples, possibly in relation with their ages and/or their places of collection.     

Elemental composition of dust in an iron foundry as determined by instrumental neutron activation analysis

In the workplace of an iron foundry total and respirable suspended particulate matter was daily collected with a network of stationary filtration systems, with Andersen cascade impactors and with personal samplers. The performances of the different sampling systems are evaluated. All samples were analysed by instrumental neutron activation analysis. More than 30 elements were determined. The composition of the particulate samples is compared to that of the major emission sources. For visualising and interpretation of the data computer programs for contour plotting, classification and clustering of the elements and the samples are applied. On the basis of their distribution and particle size the elements can be divided in a number of groups, for which easily determined elements are proposed as indicator elements. The results allow an estimate of the impact of the major emission sources on the air quality in the entire workroom. Suggestions for representative sampling techniques and locations are made.     

Radiochemical analysis of toxic elements in biological materials

A radiochemical method for simultaneous determination of toxic elements (Hg, Cd and Sb) in biological materials has been developed. The procedure involves the irradiation of samples with thermal neutrons and quantitative one-step separation in 0.1M 4-(5-nonyl)pyridine/benzene from 2.0M hydrochloric acid followed by gamma-ray spectrometry. The procedure is applied for the analysis and to the studies of distribution of these elements in IAEA-RMs, human serum and hair samples. Results obtained are found to be in good agreement with those reported in the literature.     

Multielemental analysis of soil samples by fast-neutron activation

Neutron activation analysis (NAA) have been used for the determination of major, minor, and trace elements in 20 soil samples from 5 crop fields of the Crop Research Centre, Pantnagar, India. Fast neutron activation analysis (FNAA) and cyclic neutron activation analysis (CNAA) have been used to determine the concentrations of various elements. The results for minor and trace elements are compared with the level of abundances of world soils. The present study provides the basic data of elemental concentrations in soil samples of 5 major crop fields located in one of the leading agricultural universities of India for future measurements with the objectives of efficient use of fertilizers and pesticides in accordance with the high yield.     

Inorganic trace analysis by mass spectrometry

Mass spectrometric methods for the trace analysis of inorganic materials with their ability to provide a very sensitive multielemental analysis have been established for the determination of trace and ultratrace elements in high-purity materials (metals, semiconductors and insulators), in different technical samples (e.g. alloys, pure chemicals, ceramics, thin films, ion-implanted semiconductors), in environmental samples (waters, soils, biological and medical materials) and geological samples. Whereas such techniques as spark source mass spectrometry (SSMS), laser ionization mass spectrometry (LIMS), laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS), glow discharge mass spectrometry (GDMS), secondary ion mass spectrometry (SIMS) and inductively coupled plasma mass spectrometry (ICP-MS) have multielemental capability, other methods such as thermal ionization mass spectrometry (TIMS), accelerator mass spectrometry (AMS) and resonance ionization mass spectrometry (RIMS) have been used for sensitive mono- or oligoelemental ultratrace analysis (and precise determination of isotopic ratios) in solid samples. The limits of detection for chemical elements using these mass spectrometric techniques are in the low ng g⁻¹ concentration range. The quantification of the analytical results of mass spectrometric methods is sometimes difficult due to a lack of matrix-fitted multielement standard reference materials (SRMs) for many solid samples. Therefore, owing to the simple quantification procedure of the aqueous solution, inductively coupled plasma mass spectrometry (ICP-MS) is being increasingly used for the characterization of solid samples after sample dissolution. ICP-MS is often combined with special sample introduction equipment (e.g. flow injection, hydride generation, high performance liquid chromatography (HPLC) or electrothermal vaporization) or an off-line matrix separation and enrichment of trace impurities (especially for characterization of high-purity materials and environmental samples) is used in order to improve the detection limits of trace elements. Furthermore, the determination of chemical elements in the trace and ultratrace concentration range is often difficult and can be disturbed through mass interferences of analyte ions by molecular ions at the same nominal mass. By applying double-focusing sector field mass spectrometry at the required mass resolution—by the mass spectrometric separation of molecular ions from the analyte ions—it is often possible to overcome these interference problems. Commercial instrumental equipment, the capability (detection limits, accuracy, precision) and the analytical application fields of mass spectrometric methods for the determination of trace and ultratrace elements and for surface analysis are discussed.     

Determination of elemental concentrations in environmental plant samples by instrumental neutron activation analysis

The intake of leafy vegetables in daily diet is very important to meet our nutritional needs. Vegetables provide the essential elements which are necessary and recommended for human growth. However, due to rapid industrialization and urbanization our environment becomes polluted and this affects the normal growth of agricultural products and composition of environmental species. The elemental concentrations present in the environmental samples are good indicators to assess the toxicological levels due to pollution affects. In the present work we have analysed several vegetable plant samples by instrumental neutron activation analysis to determine the elemental concentrations at major, minor and trace levels. The leafy vegetables like spinach, red leafy veagetable, pui, gourd leaf, lettuce and katoua were chosen as these are extensively consumed by local peple in eastern part of India. We have determined 15 elements in the above mentioned vegetable samples and some of these are essential elements and some are toxic elements. It was found that Na and K were present as major elements, Fe and Zn as minor elements and As, Ce, Cr, Co, La, Mo, Rb, Sc, Sm, Sr as trace elements. The concentration level of Cr was found to be higher than that of recommended value certified by WHO and National environment quality control for human consumption. The validation of our analytical results have been performed by the Z-score tests through the determination of concentrations of the elements of interest in certified reference materials.     

Neutron activation analysis of bottom and fly oil ashes

The concentrations of 25 elements in 7 oil ash samples were determinedby computerized systematic instrumental absolute neutron activation analysis.In the oil ash samples, the following mean concentrations (in ppm) of elementswere found: Al: 39531, As: 109, Ba: 1391, Ca: 29701, Ce: 295, Co: 1294, Cr:1485, Cs: 7.9, Dy: 4.5, Eu: 1.2, Fe: 53094, Ga: 146, Hf: 2.2, La: 1534, Mn:547, Na: 40277, Sb: 360, Sc: 2.3, Sm: 21, Sr: 674, Ta: 15.8, V: 130548, W:4.1, Yb: 0.9 and Zn: 3125. These findings were compared with the concentrationsof elements found in coal ash samples. The concentrations of Co, Na and Vwere significantly higher in the oil ash samples, while the concentrationof Sc was lower. The purpose of this study has been to determine the backgroundlevels of different elements in oil ash, in order to evaluate its potentialimpact on the environment.     

Neutron activation analysis of Cuban soils

Thirty elements were determined by INAA in Cuban soil samples collected in 17 zones from western regions of Cuba, which were affected by neuropathy epidemic in 1992. The presence of toxic elements was evaluated to provide data for the analysis of possible paths of intoxication through local agriculture product consumption. The results obtained for As, Th and U are compared with similar data reported on literature.