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A contemporary PM2.5 (particulate matter smaller than 2.5 microns aerodynamic diameter) aerosol material from an urban site has been collected for the production of a new standard reference material that will be made available for the development of new PM2.5 air quality standards. Air particulate matter corresponding to the PM2.5 fraction was collected at an established Environmental Protection Agency monitoring site in Baltimore, Maryland. The air-sampling system that has been constructed for this collection separates fine particles with a cyclone separator and deposits them onto an array of Teflon membrane filters. The fine air particulate material is removed by ultrasonication or by mechanical means and collected for further preparation of standards. The composition of the collected PM2.5 aerosol, as well as the composition of the deposited PM2.5 aerosol, are determined by instrumental nuclear activation analysis and other techniques.

Microbeam X-ray spectrometry, energy-dispersive X-ray fluorescence analysis, and neutron activation analysis were evaluated for the detection of selenium contained in the selenoprotein glutathione peroxidase. The glutathione peroxidase had been previously separated using polyacrylamide gel electrophoresis. The use of Bragg-reflected polarized X-ray beams was employed in the X-ray fluorescence measurements to minimize the problem of scatter owing to the gel matrix. Current detection limits of selenium in a gel matrix are 2.1 ng in the bench-top microbeam X-ray system and 30–60 ng using XRF with polarized beams. Neutron activation analysis was used for qualitycontrol measurements, with a detection limit here of

A preirradiation separation procedure has been developed to separate Al, Cu, Mn, and V from biological materials. Chelex-100 resin is used as the separation medium, and the resin is irradiated directly. Three NIST biological Standard Reference Materials and five samples of human blood serum, obtained under carefully controlled conditions, have been analyzed by NAA following this separation.

Neutron activation analysis (NAA) is an appropriate tool for the determination of trace elements in biological systems. The virtually blank-free NAA procedures fittingly complement precautions employed in sampling and sample preparation of biological matrices. Results from instrumental NAA procedures used to establish baseline values and time trends for elements in human tissues demonstrate the advantages as well as the limits of these procedures for nanomole and, in a considerable number of instances, subnanomole elemental levels. In addition, subnanomole mass fractions have been determined with extremely low limits of detection by employing NAA with radiochemical separations isolating very low levels of radioactivity from the matrix background. The elements reviewed in this article include Cr, Se, Pt, and others that have been determined by NAA at subnanomole levels in human tissues and body fluids and in biological macromolecules.

A working analytical procedure for selenium determinations by INAA, using gamma spectrometry with a germanium well-type detector, is presented. The spectral line at 400.7 keV is employed, enhanced with the effect of energy summing in true coincidence of cascade photons. The main advantage of the method is high efficiency and reliable, interference-free results; potential drawbacks are increases in input count rate and pile-up losses, decrease in resolution, and sensitivity to errors in sample-to-detector geometry. The procedure is applied to certification analysis of reference materials, large-area biomonitoring by oak leave samples, and determination of separated proteins.

Nuclear analytical techniques have an important role in the IAEA in life sciences programs relating to human health. A major effort has recently been devoted to the determination of dietary intakes of trace elements, including studies in some countries affected by the Chernobyl accident. The same accident stimulated interest in using 129I (as determined by NAA and other techniques) to trace the distribution of fission products in the environment. Other research topics concern solid wastes, air pollution, exposure to mercury in selected human populations, and osteoporosis (including NAA studies of trace elements in human bone). Much of the IAEA's work is concerned with analytical quality control; new reference materials in preparation include lichen (for trace elements) and human hair (for total and methyl mercury).

The National Institute of Standards and Technology has developed a new Standard Reference Material 1941, "Organics in Marine Sediment." In addition to the organic constituents, over 30 elements have been determined by instrumental neutron activation analysis and prompt-gamma activation analysis. The homogeneity of the material was investigated and relative standard deviations of single-element concentrations in 250-mg samples were found to be 1% or less with regard to major inorganic constituents and rare earth elements. A slightly higher relative SD was found for elements that may stem from biological or anthropogenic input. The element concentrations determined in this work are discussed in comparison to concentrations in other similar reference materials. Concentrations for 31 elements will be included for information on the certificate.

A combination of two methods, polyacrylamide gel electrophoresis (PAGE) and neutron activation analysis (NAA), has been applied to solutions containing phosphoproteins for the purpose of protein quantification. The proteins were separated by molecular weight using PAGE, and then the whole gel was activated by neutron bombardment. Densitometric measurements of the developed bands from 32P, taken from autoradiographs of the activated gels, resulted in quantification of the phosphorus, and then the related protein. This PAGE/NAA method was applied to several phosphoprotein- containing materials, including commercial milk products and reference materials, i.e., IAEA A-11, milk powder, and SRM 1845, Cholesterol in Egg Powder.

A project to establish an archive of Alaskan marine mammal tissues was conceived in 1987 to be a part of the National Biomonitoring Specimen Bank (NBSB). Protocols and field collection of marine mammals, long-term storage, and analysis are summarized in this paper. Instrumental neutron activation analysis has been used for an initial evaluation of trace element content in samples of northern fur seal (Callorhinus ursinus) from the Pribilof Islands. The findings agree with previously observed trace element levels in northern fur seals. The archived specimens can be used in future studies when comparison of past and present pollution levels are needed.

The validity and intercomparability of data in research related to medical, environmental, and geochemical health problems is of utmost concern and requires specific consideration in the development of an analytical approach. The Environmental Protection Agency/National Bureau of Standards Pilot Environmental Specimen Bank Program provides a vehicle for developing the precise and accurate determination of trace constituents in human livers. This approach, when implemented, gives specific consideration to a valid relationship between the analytical result and the true value in the sample. This is accomplished by minimizing contamination of the sample and/or loss of constituents, and by assuring representative analytical test portions. The analysis of the liver specimens is performed under strict quality control. The applied analytical techniques (atomic absorption spectrometry, isotope dilution mass spectrometry, neutron activation analysis, and voltammetry) have been verified for accuracy through the analysis of Standard Reference Materials. In addition, several elements are determined using two or three of these independent techniques. The first year of the program provided results on 31 elements including Se and Pb in 36 human livers.