Multi-elemental characterization of Cuban natural zeolites

Concentrations of 38 elements in samples from four important Cuban zeolite beds have been obtained by Instrumental Neutron Activation (INAA) and X-ray Fluorescence analyses (XRFA). In comparison with other analytical techniques good agreement was reached. The concentration values of minor element Ba, Sr, Zn and Mn and 25 trace element (including 9 REE) are at the first time reported in Cuban zeolite. It is important for the zeolite evaluation in different industrial uses.     

Study on air pollution monitoring in Korea using low volume air sampler by instrumental neutron activation analysis

The aim of this research was to enhance the use of nuclear analytical techniques for air pollution studies and to study the feasibility of the use of instrumental neutron activation analysis (INAA) as a routine monitoring tool to reveal environmental pollution sources. For the collection of air particulate samples, the Gent stacked filter unit, low volume sampler with Nucleopore membrane filters were used. Trace elements in samples collected at two suburban residential sites, Taejon and Wonju city in the Republic of Korea, were analyzed by INAA. Variations of the elemental concentrations were measured monthly and the enrichment factors were calculated for the fine (<2 μm EAD) and coarse size (2–10 μm EAD) fractions. The analytical data were treated statistically to estimate the relationship between the two variables, the concentrations of elements and the total suspended particulate matter. The results were used to describe the emission source and their correlation.     

Study on air pollution monitoring in Korea using instrumental neutron activation analysis

Trace elements in airborne particulate matter collected monthly at suburban and rural areas in Korea were analyzed by instrumental neutron activation analysis (INAA). Neutron irradiation of the samples was done at the irradiation hole (neutron flux 1·10¹³ n·cm^–2·s^–1) of the TRIGA Mark-III Research Reactor in the Korea Atomic Energy Research Institute. For the verification of the analytical technique, two reference materials, NIST SRM-1648 and NIES CRM-8, were chosen for analysis. The accuracy and precision of the determinations of the 40 elements were compared with the reference values. We used this method (1) to analyze 30 trace elements in airborne particulate matter collected monthly with the high volume air sampler (PM-10) at two different locations and (2) to confirm the possibility of using this method as a routine monitoring tool to find out environmental pollution sources.     

Application of two INAA methods to pollution studies of sediments from Saronikos Gulf,Greece

Thirty elements were determined by two INAA methods in sediment core samples from N. Saronikos Gulf, Greece, and the results were subjected to multivariate analysis. This procedure resulted in the separation of samples into chemical groups that were environmentally meaningful and sufficient to (a) distinguish among different pollution sources; (b) trace the routes and the extent of pollution in sediments; and (c) define the least affected areas representing the geochemical background. The principal components analysis of the analytical data for 18 selected elements revealed that, among the elements determined in this study, the most discriminating were As, Sb, Ag, Ca, Au, Zn and the rare earth elements (REE).     

Determination of Elements in Japanese Standard Soil Materials by Means of Insturmental Neutron Activation Analysis

Instrumental neutron activation analysis (INAA), and inductively coupled plasma mass spectroscopy (ICP-MS) were applied to the determination of major elements and rare earth elements in Japanese Standard Soil Materials (NDG-1 to -8). Eight major elements, Al, Fe, Ti, Ca, Mg, Mn, K, and Na were determined by INAA. A comparison of the data for rare earth elements obtained by INAA and ICP-MS shows that the data of the contents determined by the two different analytical methods are in fairly good agreement with each other.     

Determination of trace impurities in electronic grade quartz: Comparison of inductively coupled plasma mass spectroscopy with other analytical techniques

An analytical procedure for the determination of uranium and thorium in the sub-ng/g range as well as of other trace elements in the ng/g to g/g range in high purity quartz samples is described. The results obtained by inductively coupled plasma mass spectroscopy (ICP-MS) are compared to those obtained by other analytical techniques (instrumental neutron activation analysis, INAA; flame atomic absorption spectrometry, AAS; Zeeman graphite furnace atomic absorption spectrometry, ZGFAAS; total reflection X-ray fluorescence analysis, TRFA; direct current arc optical emission spectrometry, DC-arc OES; and X-ray fluorescence analysis, XRFA). For the ICP-MS measurements, the decomposition of the samples is carried out with HF/HNO₃/H₂SO₄-mixtures. The results obtained by the different methods show reasonable agreement. For uranium and thorium, ICP-MS proves to be the most sensitive method: detection limits of about 50 pg/g can be achieved for both elements.Presented in part at the 1989 European Winter Conference on Plasma Spectrochemistry, Reutte, Austria     

Multielemental neutron activation analysis of fugitive dust particulates from cement factories in Central India

Knowledge of occurrence and concentration of trace elements in dust particulates from and around industrial establishments is essential to know the source of pollutants and atmosphere quality. Dust particulates from two cement factories in the central part of India were analyzed for 5 minor (Cl, Fe, K, Mg, Na) and 23 trace elements (Ag, As, Ba, Br, Cd, Co, Cr, Cs, Dy, Eu, Ga, Hf, Hg, La, Mn, Sb, Sc, Se, Sm, Sr, Th, W and Zn) by INAA and RNAA techniques. Significant differences have been observed for some toxic trace elements at different locations. Mn content is particularly high in all the dust particulates. Urban particulate (SRM 1648) and Coal fly ash (SRM 1633a) from NIST and Pond sediment (CRM No. 2) from NIES were also analyzed. The data have been analyzed and interpreted in terms of air quality at different locations inside the plant and two factories.     

Determination of trace elements by INAA in urban air particulate matter and transplanted lichens

Summary Lichens as biomonitors and neutron activation analysis as analytical technique have been employed to evaluate the trace element atmospheric pollution in the metropolitan area of the city of Pavia (Northern Italy). Transplanted lichens (Parmelia sulcata and Usnea gr. hirta) and air particulate matter have been monthly collected and analyzed during the winter 2001-2002. INAA and ET-AAS have been used for the determination of 28 elements in air particulate matter and 25 elements in lichens. Trace metals concentrations as well as the corresponding enrichment factors were evaluated and compared.     

Nigerian coal analysis by PIXE and RBS techniques

PIXE and RBS techniques were employed for the measurement of the concentrations of the major, minor and trace elements in Nigerian coal samples from a major deposit. The samples were irradiated with 2.55 MeV protons from the 3 MeV tandem accelerator (NEC 3 UDH) in Lund. The PIXE results are reported and compared with an earlier work on Nigerian coal using FNAA and INAA analytical techniques while the RBS results are compared with ASTM previous results. The results show that Nigerian coals have a low (0.82–0.99)% sulfur content. This is quite important for pollution control reasons.     

A contribution to the certification of some elements in eight vegetal reference materials by using instrumental neutron activation analysis

Instrumental neutron activation analysis (INAA) has been applied to the determination of 21 elements in 8 different vegetal samples, to be used as reference materials in 35 European laboratories (CII). Many of these elements hitherto have not been evaluated; they can be useful markers in many environmental problems. The INAA values are compared with CII non-nuclear analytical techniques results. Some rare earths elements (REE) have been also determined and their chondritic ratio versus atomic radius is reported.     

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.     

Foliar contamination and uptake from aerial sources investigated by INAA and XRFA

The suitability of standard grass as bioaccumulator for different elements was investigated theoretically as well as experimentally using INAA and XRFA. The calculation is based on the annual mean values of elemental mass concentration in air at three sites with various characteristics and on the published data for deposition velocity. The potential contaminations computed in this way and supported by our experimental results were compared with the average mass contents in the standard grass. The resulting degrees of potential contamination show that for elements as Cr, Fe, Hg, Pb and Sb the monitoring with standard grass is normally possible, while for other elements (e.g. Br, Ca, Co, K, Mn, Na, Ni, S, Zn) the separation of contamination by film stripping method is indispensable. There is also an intermediate group (As, Ba, Se).     

Standard Reference Materials® (SRMs) for measurement of inorganic environmental contaminants

NIST has developed an extensive collection of environmental SRMs, starting with fuel and biologically related materials in the late 1960s and now encompassing all sectors of environmental research. Advances in analytical methodology, including multi-element isotope-dilution mass spectrometry (IDMS) and expanded instrumental neutron-activation analysis (INAA) capabilities, enable value assignment based on fewer but better-characterized independent analytical techniques. The special advantages of IDMS for determination of S and Hg and for multi-element characterization of small-sample air particulate matter (SRM 2783) by IDMS and INAA are emphasized. Developments in materials production include the issuance of fresh-frozen biological materials and of jet-milled natural-matrix materials with improved homogeneity, including highly homogeneous air particulate matter and sediment SRMs for small-sample analytical techniques.     

Neutron activation analysis: Still a reference method for air particulate matter measurements

At ITN, PM10 and PM2.5 aerosols were collected on Nuclepore^® polycarbonate filters of 47 mm diameter, using Gent samplers at 15–17 l/min air flux. Filters were analyzed by INAA and PIXE. The availability of certified filters was very scarce, viz.: (1) fly ash embedded in a methyl cellulose 47 mm foil 10 µm thick, BCR CRM128, (2) particle-size reduced air particulate matter (APM) to simulate PM2.5 aerosol matter deposited on a 47 mm polycarbonate filter membrane, NIST SRM 2783. The high price and scarcity of APM standards did not permit their frequent use for analytical quality control. At ITN, to control the filter results' accuracy, the chemical elements potassium, iron and zinc, determined by both techniques, were systematically compared. After a few improvements introduced in INAA, this technique was now considered at ITN as the reference technique in air particulate measurements. Comparison of INAA to PIXE was discussed. Compared to previously reported situation it was concluded that the results were in better agreement for iron and zinc, and potassium values were still biased to the same extent as before.     

A review on activation analysis of air particulate matter

A review is presented on the use of various activation analysis methods for the determination of trace elements in air particulate and related matters. A discussion is given on the contribution of such methods in solving the problem of air pollution in various parts of the world. This work is a part of a program undertaken by this Department for the evaluation of the various analytical techniques as investigative tools in pollution and other environmental studies.     

Excitation functions and energy spectra of proton induced reactions on56Fe and57Fe in the energy up to 30 MeV

The atmospheric particulate of industrialized cities had become a mixture of potentially toxic substances whose concentrations must be monitored to assess the pollution levels. Trace metals and elements are part of these pollutants and the knowledge of their total concentration in the air as well as their distribution in the different aerosol particle sizes is necessary to evaluate the pollution risk in terms of maximum present levels and long term exposure. In the present work, a preliminary part of a study initiated for monitoring the trace element levels present in the atmospheric particulate of the city of Milan (north Italy) and of its suburban areas is presented. More than 25 elements have been determined in Milan downtown along a period of three years and in different weather conditions. The granulometric distribution of selected potentially toxic elements (such as vanadium, lead, cadmium, nickel) has been also determined to evaluate their concentrations in different inhalable fractions (alveolar and bronchial — tracheal). Instrumental Neutron Activation Analysis (INAA) has been used for the determination of the great part of the elements while Graphite Furnace Atomic Absorption Spectroscopy (GF-AAS) has been employed for the determination of lead and, in some cases, for nickel, cadmium and copper.     

Use of INAA,PGAA, and RNAA to determine 30 elements for certification of an SRM: Tomato Leaves, 157a

Analyses for certification have been made for the determination of 30 elements in the National Institute of Standards and Technology (NIST) Tomato Leaves renewal reference material, SRM 1573a. Three of the analytical techniques used were instrumental neutron activation analysis (INAA), radiochemical neutron activation analysis (RNAA), and prompt gamma activation analysis (PGAA). These techniques provided data on 19 elements by INAA, 10 elements by PGAA, and 7 elements by RNAA, with some overlap between techniques. For example, INAA was able to obtain overall analytical uncerainties (at the 95% confidence level) averaging ±2.2% for major and minor constituents (Ca, Mg, K), ±3.3% for constituents from 1 to 1000 g/g (Na, Fe, Al, Mn, Ba, Zn, Rb, La, Cr), and ±6.4% for elements between 10 and 1000 ng/g (Co, V, Se, Th, Sc, Sb), using sample dry weights of approximately 150 mg. These analyses represent the most extensive use to date of nuclear analytical techniques in the certification of a trace element SRM at NIST.     

Determination of the elemental contents in stream sediments collected from Cheongju city by instrumental neutron activation analysis

Sediment samples were collected from seven locations of the MeeHo stream in Cheongju city, strained out by a sieve, dried by an oven and pulverized by an agate mortar. Instrumental neutron activation analysis (INAA) was applied for the determination of the elemental contents in the sediment samples by using the NAA #1 and #2 irradiation holes of the HANARO research reactor and HPGe gamma-ray spectrometers. Twenty-five elements were determined by a relative method with NIST SRM 2711-Montan Soil and the ranges of the elemental contents for the seven locations were identified. The contamination levels for elements such as As, Ba, Cr, Mn, Fe and Zn were compared with the guidelines of USEPA. The detection limits and combined uncertainties for the hazardous elements such as As, Ba, Cr, Mn, Sb, V and Zn were estimated under the given analytical conditions.     

Critical review on the development of analytical techniques for the elemental analysis of airborne particulate matter

Among all environmental pollutants, particulate matter (PM) poses the major threat to our health. These tiny airborne particles vary in shape and composition, which is reflected in their hazardous potential. The particles are small enough to penetrate deep into the lungs and even enter the bloodstream, causing severe diseases. Therefore, their regular monitoring is required. Toxic metals and other elements are often measured by regulatory agencies as well as in research laboratories, either to compare ambient concentrations with prescribed limit values or to study provenance of air pollution sources in order to target PM pollution mitigation strategies. The most established method for the determination of regulated Pb, Cd, As, Ni and other elements in PM is microwave digestion inductively coupled plasma mass spectrometry (MW/ICPMS), whereas X-ray fluorescence (XRF) techniques have also often been used, especially in research. In this review paper we critically assess these two and three other analytical techniques (i.e., LA-ICPMS, PIXE and INAA) for element determination in PM deposited on filter media. All aspects from sample treatment to measurement range and limitations, costs and waste management are considered. In conclusion we identify XRF and LA-ICPMS as two promising surface techniques for the analysis of a PM deposit on a filter, which could replace the laborious wet MW/ICPMS method, which is – considering its wide use, very incriminating to the environment. In short, EDXRF is the cheapest, simplest for use and already customized for PM samples, whereas LA-ICPMS is promising, but still needs some development in the direction of autosamplers and matrix-matched standards for calibration.     

Application of instrumental neutron activation analysis and inductively coupled plasma-mass spectrometry to studying the river pollution in the State of Minas Gerais

Instrumental neutron activation analysis (INAA) and inductively coupled plasma-mass spectrometry (ICP-MS) have been used for the determination of toxic heavy metals and other pollutants in the water of the Das Velhas river in the State of Minas Gerais, in south-east Brazil. Elemental concentrations of about 60 elements were measured in water samples collected to different parts of this river and from two affluents. There was a good agreement between the two analytical methods and the results were complementary. The results indicated an increase in the concentration of several polluting elements in the water from mining industry area.