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Instrumental neutron activation analysis may need to correct for matrix interferences caused by fast neutron induced threshold reactions. The very low Al mass fraction in bovine liver Standard Reference Material (SRM) has eluded certification due to such complications. Cold neutron beam irradiation absent fast neutrons provides a possible alternative, which has been applied for the first time to determine Al in bovine liver SRM 1577c. The Al mass fraction was determined to be (0.80 ± 0.15) mg/kg using the traditional single peak-fitting method, and (0.78 ± 0.23) mg/kg using a new physics model-based spectral fitting method.

We have established an instrumental neutron activation analysis (INAA) method, including k0-based INAA, at the Korea Research Institute of Standards and Science (KRISS) for the certification of reference materials. As part of establishing INAA measurements, KRISS infant formula certified reference material was analysed for multiple elements at three different metrological institutes: KRISS and NIST for the standard comparator method, and JSI for the k0-INAA method. The mass fraction of most elements was consistent within expanded uncertainty (k = 2). In addition, the results were used to verify the validity of elemental analysis of Zn using the standard comparator INAA at KRISS, and spreadsheet-based INAA calculations were evaluated.

An innovative reference material of sugarcane leaves with homogeneity demonstrated for masses greater than 50 mg for major, minor and trace elements was developed at CENA/USP, Brazil. INAA and PGAA were chosen for the final chemical characterization at the NIST Center for Neutron Research. INAA allowed the determination of twenty elements, while PGAA allowed the determination of B, Cl, Fe, K, Mn, N and Si. Similar mass fraction values were obtained for those elements determined by both nuclear techniques in the sugarcane leaves reference material, as well as in SRM1570 and SRM1572.

A new γγ coincidence system has been set up at NIST. It is operated with a digital data finder supported by new software developed at NIST. The system is used to explore possible enhancements in instrumental neutron activation analysis (INAA) and study applicability to neutron capture prompt gamma activation analysis (PGAA). The performance of the system is tested with certified reference materials for efficiency calibration and quantitative performance. Comparisons of INAA results based on conventional gamma-ray spectrometry data with INAA results based on coincidence data obtained from the same samples show improvements in the counting uncertainties and demonstrates the quantitative accuracy of the new system.

Instrumental neutron activation analysis (INAA) and prompt gamma neutron activation analysis (PGAA) were used to characterize a variety of single-wall carbon nanotube (SWCNT) materials from different principal production processes, as well as a material containing SWCNTs together with other carbon species, catalyst residues, and trace element contaminants to be issued by the National Institute of Standards and Technology for characterization and distribution as Standard Reference Material SRM 2483 Carbon Nanotube Soot. INAA proved to be well suited for the direct determination of catalyst and contaminant trace elements requiring only minimal sample preparation. PGAA complemented the INAA data in particular with determinations of the light elements. Carbon and hydrogen results provided information on the materials purity and storage properties. Strategies for the quality assurance of the measurements in these new materials were developed. INAA and PGAA data were provided for the value assignment of mass fractions of catalyst and trace elements in the candidate SRM and a systematic overview was obtained of the catalyst and trace element contaminants associated with each of the major production routes.

A combination of instrumental neutron activation analysis (INAA) and prompt gamma-ray activation analysis (PGAA) was used to value assign 35 elements in SRM soil 2709a (San Joaquin Soil). INAA with counting of short-lived radioisotopes was used for determination of Al, Au, Ca, Dy, K, Mg, Mn, Na, Ti, and V. Elements determined by INAA with counting of intermediate and long-lived radioisotopes included As, Ba, Ce, Co, Cr, Cs, Eu, Fe, Hf, La, Lu, Nd, Rb, Sb, Sc, Sm, Sr, Ta, Tb, Yb, Zn, and Zr. Thermal neutron PGAA was used for the determination of H, B, Si, K, Ti, Mn, Fe, Cd and Gd. Expanded uncertainties were determined for all values reported.

Instrumental neutron activation analysis as carried out at the National Institute of Standards and Technology (NIST) is inadequate for determining Al, Ni, and V at the levels found in the newly prepared Standard Reference Material® (SRM) 1577c Bovine Liver. To overcome shortcomings in the value assignment, the authors initiated a cooperative approach using NAA with previously established chemical separation procedures and with significantly different neutron energy spectra to determine Al and V with pre-irradiation separation of the elements at NIST, and V and Ni with post-irradiation separation at the Nuclear Physics Institute Řež. The determinations were confirmed with the analyses of several SRMs. The work supported the certification of mass fraction values for V and Ni in SRM 1577c.

Cold neutron prompt gamma activation analysis (PGAA) was used to determine the mass of hydrogen in Mg hydride thin films with varying hydrogenation times. The results suggest that hydrogenation of the Mg thin films remains unsaturated even after 48 h of treatment, contrary to the indications of inferential hydrogen measurement methods. To demonstrate PGAA as an effective combinatorial methodology for hydride thin films, a continuously varying composition gradient of thin MgyTi(1−y) hydride film with y ranging from 0.65 to 0.94 was prepared and analyzed by both PGAA and instrumental neutron activation analysis (INAA). The variation in the molar ratio of Mg, Ti, and H was obtained for nine 5 mm wide segments of the film.

Analyses for value assignment in the renewal Standard Reference Materials® SRM 1598a Animal Serum and SRM 1577c Bovine Liver included extensive characterization by neutron activation analysis (NAA). Conventional instrumental NAA procedures were complemented by pre-irradiation chemical separations for the determination of Al, V, Mn, and Cu, radiochemical separations for the determination of Ag, As, Cd, Cr, Cu, Mo, Sb, and Se, and the use of (anti-) coincidence gamma-ray spectrometry systems for the instrumental determination of Ag, Cr, and Hg. The previous materials, SRMs 1598, 1577, and 1577b, were analyzed together with the new materials for quality control.

The National Institute of Standards and Technology (NIST) is preparing a freeze-dried powdered bovine liver tissue Standard Reference Material (SRM) to replace SRM 1577b Bovine Liver as the stock of this material was exhausted during 2006. Like the original SRM 1577 issued in 1972, this renewal focuses on the key elements for diagnostic, nutritional, and toxicological measurements that are important to medical, veterinary, and environmental sciences investigations. NIST’s approach for value assignment included extensive characterization by neutron activation analysis (NAA). Difficulties in the determination of some elements present at very low levels were overcome by use of radiochemical separations. Twentyone elements were characterized in SRM 1577c by NAA. The previous materials, SRM 1577 and 1577b, served as quality control.

For accurate activation analysis, it is necessary to understand the neutron and gamma-ray environment experienced by a sample during irradiation. A new irradiation position was recently installed in the RT2 thimble of the NIST reactor. Modeling by MCNP was used to select the radial location in the reflector thimble and the size of the D2O shielding tank. After installation, the new rabbit was characterized for thermal, epithermal, and fast fluence rates, spectral parameters f and α, temporal stability, axial and radial flux gradients, and temperature.

The basic assumptions of activation analysis are that the induced radioactivity is proportional to the amount of analyte, and that the quantity of radioactivity can be related simply to the number of counts observed. Quantitative measurement of activity (and of its uncertainty) is not always simple, especially when accuracy better than a few percent is sought. Recent work with 77Ge and 76As has demonstrated that the accuracy of half-lives in the literature is sometimes insufficient. Despite these and other problems, quantitative understanding and documentation of uncertainties can be accomplished, providing demonstrable quality assurance and supporting claims of traceability to the Systeme International.

The determination of arsenic at natural levels in biological materials remains difficult. Many analytical techniques cannot detect the low levels present in typical biological tissues and other techniques suffer from interferences. This paper reviews uses of neutron activation analysis (NAA) at NIST to determine nanogram amounts of arsenic in biological reference materials with radiochemical (RNAA) or instrumental (INAA) procedures. INAA is compromised by high activities from 24Na, 82Br, and 32P that may be formed during irradiation of biological tissues, and result in detection limits as high as 0.1 mg. Lower detection limits have been achieved using state-of-the-art gamma-ray spectrometry systems in INAA and a variety of procedures in RNAA. These techniques and procedures were applied recently at NIST to the determination of arsenic in urine, nutritional supplements, and total diet samples.

A new radiochemical neutron activation analysis (RNAA) method has been developed for low-level determination of Si in biological materials, which is based on the 30Si(n,γ)31Si nuclear reaction with thermal neutrons. The radiochemical separation consists of an alkaline-oxidative decomposition followed by distillation of SiF4. Nuclear interferences, namely that of the 31P(n,p)31Si with fast neutrons, have been examined and found negligible only when irradiation is carried out in an extremely well-thermalized neutron spectrum, such as available at the NIST reactor. The RNAA procedure yields excellent radiochemical purity of the separated fractions, which allows the measurement of the β--activity of the 31Si by liquid scintillation counting. Results for several reference materials, namely Bowen’s Kale, Bovine Liver (NIST SRM 1577b), Non-Fat Milk Powder (NIST SRM 1549) and several intercomparison samples, Pork Liver-1, Pork Liver-2 and Cellulose Avicel, are presented and compared with literature values.

This work provides a systematic experimental approach to the demonstration of viability of instrumental neutron activation analysis (INAA) in chemical metrology. The practical approach was derived from a complete survey of uncertainty components that affect the INAA measurement process. These uncertainty components were classified by their magnitude and origin and subsequently minimized by appropriate steps in the INAA process. The process was tested with the INAA determination of Cr in SRM 1152A stainless steel; the Cr value is certified at 17.76% with an estimated uncertainty of 0.04% (0.23% relative). The INAA results from this procedure are in agreement with these specifications. Similar procedures have been applied to INAA multi-element determinations in a high temperature alloy. Agreement with available consensus values was demonstrated in the alloy. The guidelines on the determination of uncertainty were fully met, providing through INAA a valuable independent non-destructive tool in chemical measurements of metrological value such as required in the CCQM key comparisons.

The optimization of neutron activation analysis with regard to detection limit and uncertainty of measurement using physical and chemical means is reviewed. Using selected examples it is demonstrated that radiochemical separation is the most effective means of optimization, especially in neutron activation analysis, because it yields the lowest detection limits and uncertainties.

A novel approach is implemented to alleviate some persistent problems in neutron capture prompt gamma activation analysis (PGAA). Detection sensitivities of PGAA are often restricted by the following factors: poor signal to noise ratios, interferences from background signals, and, in some cases, overlapping energy lines from different origins, namely ultra short-lived decay lines interfering with prompt decay. Timing the gamma-ray acquisition with the actual capture events using a pulsed beam of cold neutrons allows discrimination between prompt and delayed emissions from a sample source as well as against background events. Coincidence gating selects the prompt gamma-ray emissions. Contributions of background capture gamma-rays are suppressed because of different flight times of neutrons to the sources of background radiation, providing a reduction in direct gamma-ray interferences. Anti-coincidence gating allows measurement of only decay radiation that originates from short-lived activated states of the nuclides after capture. Spectra of decaying nuclides are free of interfering prompt activities, as well as have lower continuum background from Compton scattering of high-energy prompt gamma-rays in the detector. The measurements provide the opportunity to use ultra-short half-life nuclides for analytical purposes, no sample transfer times are lost, and repetitive activation and counting cycles are achieved with the use of pulsed neutron beams.

A fast (14-MeV) neutron activation analysis procedure was employed to directly measure mass fractions of oxygen in coal samples. The procedure demonstrated sufficient precision and accuracy to determine a relative change of about 5% or more, in the oxygen mass fraction of about 12%. The procedure was applied to test samples of the newly developed SRM 1632c Trace Elements in Coal (Bituminous). The samples had been stored at three conditions: in liquid nitrogen vapor and at room temperature in the original containers packaged under argon, and for accelerated aging at 50 °C open to air. Following six months storage increments, duplicate samples of each of twelve bottles of the SRM were measured for each storage condition. In addition each sample was processed through ten separate analytical runs yielding a total of some 720 measurements per storage duration. Oxygen was determined by comparison to a primary standard potassium dichromate and the accuracy of the method was assessed through the analysis of replicate samples of three reference materials that are certified for oxygen content. The initial 6-months test period indicated uptake of oxygen in the open-air storage.

Instrumental neutron activation analysis (INAA) procedures were optimized for the analysis of small (1 mg) solid samples. This process included sample handling as well as detailed evaluation of high rate counting techniques, also in conjunction with rapidly decaying sources, to establish the necessary analysis environment for the determination of large numbers of samples with high reproducibility. The investigated materials included biological materials such as peach leaves (SRM 1547), lichen, and bovine liver, as well as environmental materials such as urban particulate matter (SRM 1648), and deep ocean sediment. The analytical data obtained with the INAA procedures were used to determine homogeneity values.

Gamma-ray spectrometry losses through pulse processing dead time and pile-up are best assayed with an external pulse technique. In this work, the virtual pulse generator technique as implemented commercially with the Westphal loss free counting (LFC) module is set up and tested with four high resolution gamma-ray spectrometers. Dual source calibration and decaying source techniques are used in the evaluation of the accuracy of the correction technique. Results demonstrate the reliability of the LFC with a standardized conventional pulse processing system. The accurate correction during high rate counting, including during rapid decay of short lived activities, has been the basis for highly precise determinations in reference materials studies.

Instrumental neutron activation, proton induced X-ray emission and energy-dispersive X-ray fluorescence procedures were employed for trace element determinations in samples of fractionated air particulate matter deposited on filters. The techniques are well suited to analyse the generally small samples. However, indications of bias between techniques were found in the analysis of individual filters. This may be rectified with the development of matched reference materials. The three techniques were used in this work to determine trace elements in bulk samples of air particulate matter and in a set of intercomparison samples of fine air particulate matter on filters. The test results on these materials showed good agreement among the employed techniques and demonstrated the quality potential of air particulate analyses.

Arsenic (As) is widely found in marine organisms, mainly as organic arsenical compounds. With the introduction of regulations for As species in foodstuffs and for environmental control, it has become more important to quantify the amount of arsenic species present. To address this concern new reference materials (RMs) for validation and quality assurance of As speciation measurements are being developed, including a tuna fish tissue and a robalo liver tissue. Instrumental neutron activation analysis (INAA) is used in this work as a proven analytical tool for As determinations and for validating the As mass fraction determined by liquid chromatography coupled to inductively coupled mass spectrometry (LC–ICP-MS) in extracts of the candidate RMs and other fish samples including certified RMs. Various methods for the extraction of water-soluble As species were evaluated. The best results were acquired after methanol/acetone/water extraction yielding in 93 % extractable As in the tuna RM. This procedure was used for the LC–ICP-MS studies. The results demonstrate that INAA can account for 100 % of the distribution of As species in analytical processes. It complements LC–ICP-MS for the validation of the characterization of As species in the development of RMs for such species. Excellent agreement of measured results in certified RMs with the reported values confirms the validity of the applied procedures.

The most important fraction of aerosols with respect to human health is the respirable fraction, which has particles less than 10 μm in equivalent aerodynamic diameter (EAD), the so called PM 10 fraction. The collection of these respirable particles and the determination of their trace element composition is the focus of an IAEA Co-ordinated Research Programme (CRP). The IAEA Laboratory participated in this Programme and established collection sites for the air particulate samples on the grounds of the Atominstitute of the Austrian Universities in Vienna and the IAEA Laboratories, Seibersdorf, representing an urban residential site and a rural site. The collected samples as well as samples of simulated air filters (used also for blind controls) and control materials were analyzed sequentially and/or in sections by X-ray fluorescence (XRF), proton induced X-ray emission (PIXE), instrumental neutron activation analysis (INAA), and atomic absorption spectrometry (AAS). Results demonstrate the applicability of the PM-10 sampling approach, provided PIXE and/or INAA are used in the determinations. Reliable results can be obtained that will lead in comparable air pollution data for many regions in the world through CRP.

A simple radiochemical procedure has been developed to separate lead and polonium simultaneously from different environmental and biological materials. After adding 208Po tracer and lead carrier samples are decomposed using mineral acids. Lead and polonium are selectively retained from 2m HCl solution by the bis-4,4′(5′)-t-butyl-cyclohexano-18-crown-6-ether; polonium is stripped with 6 m HNO3 while lead is stripped with 6 m HCL solution. A polonium source is prepared by spontaneous deposition onto a silver disk. The activity concentration of 210Po is determined by isotope dilution alpha spectrometry. Lead is precipitated as oxalate; the chemical recovery is determined by gravimetry. The activity concentration of 210Pb is calculated from the liquid scintillation spectrum.

At the end of the 1991 Gulf War the U.N. Security Council Resolution called upon IAEA, assisted by the U.N. Special Commission, to carry out inspections of all Iraqi nuclear installations. The IAEA Action Team succeeded in implementing, on very short notice, a comprehensive system of inspection activities, including sampling and analysis at the Agency's Laboratories and other laboratories in Member States. The Agency's Laboratories developed and implemented an analytical strategy with the aim to rapidly and accurately obtain the information necessary for verifying the Iraqi declarations. The analyses ranged from screening for α- and β/γ-emitters to accurate determinations of the amounts and isotopic composition of the radionuclides and associated trace elements and compounds. The arsenal of methods included ultra-sensitive radiometric methods, mass spectrometry, neutron activation, X-ray fluorescence and inductively coupled plasma emission spectrometry. Selected results include the detection of uranium chloride compounds, special composition steels, and quantitative accounting of uranium and plutonium production. The selectivity, sensitivity and reliability of the applied analytical techniques in conjunction with validated sampling procedures are essential components of an analytical measurements system that can provide credible results.

A source of error in the gamma-spectrometric registration of the analytical signal in neutron activation analysis is its dependency on the overall count rate. Losses in the accuracy of quantitation occur due to hardware and software. This paper presents examples for solutions to these problems and demonstrates that accurate NAA can be accomplished under high-rate counting conditions with commercially available technology.

Two new materials are introduced that might serve as useful aids for the harmonisation of analytical results. Spruce shoots, cryogenically homogenized and characterized for 50 elements from two sampling sites of the German Environmental Specimen Bank (ESB) are presented as possible third generation reference materials that might also act as calibrating materials in speciation analysis.

The cryogenic archival of biological specimens for retrospective analysis is of significant value for present and future research on population genetics, pathology, systematics, toxicology and environmental monitoring. This realization is emphasized by the increasing support of this activity by various government agencies, institutions and international groups. The international Arctic community is no exception. Canada has been conducting such activities in association with environmental monitoring programs for many years. Similar efforts appear to be underway in other polar nations. From the perspective of the United States Arctic, the Alaska Marine Mammal Tissue Archival Project (AMMTAP) was the earliest organized effort to develop an environmental specimen bank specifically designed for longterm archival of biological specimens under cryogenic conditions. The AMMTAP emphasizes use of standardized rigorous sampling and archival protocols, procedures that minimize contamination of samples during collection and maintaining a detailed record of sample history. The development of this specimen bank, recent activities of this project and other cryogenic specimen banks being developed in Alaska are described.

The feasibility of performing immunoassays with colloidal gold labels and detection of198Au by neutron activation has been demonstrated with measurements of human immunoglobulin and of serum antibodies to human immunodeficiency virus type 1. The detection sensitivity achieved after activation in a high flux reactor or with a water moderated252Cf source, by gamma-counting or by autoradiography, is similar to the sensitivity obtained with absorbance measurements in the more common enzyme immunoassays. The reactor based neutron activation assay allows detection of 10−16 mol of analyte in routine operation with possible extension to 10−20 mol. The sensitivity with the 1.3 Ci252Cf source is limited to about 10−15 mol. The practical limitations of the assay's sensitivity at this point are due to background signals from reagents and/or nonspecific binding of the gold labeled reagent.

An instrument for neutron capture prompt gamma-ray activation analysis (PGAA) has been constructed as part of the Cold Neutron Research Facility at the 20 MW National Institute of Standards and Technology Research Reactor. The neutron fluence rate (thermal equivalent) is 1.5·108 n ·cm−2·s−1, with negligible fast neutrons and gamma-rays. With compact geometry and hydrogen-free construction, the sensitivity is sevenfold better than an existing thermal instrument. Hydrogen background is thirtyfold lower.

Instrumental neutron activation analysis (INAA) has been employed in the investigation of mass balance for mercury species analysis in the analytical process. A new human hair reference material (IAEA-085) was analyzed for methylmercury using a solid/liquid extraction procedure, with samples of extracts, residues, and untreated samples being analyzed by INAA. The certified reference material NIES CRM No. 13, human hair, was analyzed in parallel. From the results obtained through the mass balance studies, it was found that the extraction procedure was quantitatively complete, and that there was no difference between the mass balance of Hg and the total Hg in the untreated materials.

Analyses of selected tissues from the Alaska Marine Mammal Tissue Archival Project (AMMTAP) have provided comprehensive information related to levels of 36 trace elements and methyl-mercury in marine mammal tissues. Liver, kidney and muscle tissues from two northern fur seals, four ringed seals and six belukha whales were analyzed. The bulk of the investigated tissues and additional tissues from a total of 65 marine mammals are banked in the AMMTAP. The results are compared to literature values for trace element concentrations in marine mammal tissues and their relevance to environmental studies is discussed.

The National Institute of Standards and Technology (NIST) has been involved in biological environmental specimen banking activities since 1979. These activities, which are known collectively as the National Biomonitoring Specimen Bank (NBSB), include the banking of a variety of specimens (human liver, sediment, mussels/oysters, fish tissue and marine mammal tissues) from several different projects supported by different government agencies. The two most recent projects, the Alaska Marine Mammal Tissue Archival Project (AMMTAP) and the National Marine Mammal Tissue Bank (NMMTB), focus on the collection, banking and analysis of marine mammal tissues and they are part of a comprehensive plan to address marine mammal monitoring, specimen banking and quality assurance of analytical measurements associated with contaminant analyses in marine mammals.

The National Biomonitoring Specimen Bank at the National Institute of Standards and Technology applies a variety of techniques for extensive characterization of banked samples. To determine a large number of trace elements in small samples at low levels, instrumental neutron activation analysis has been combined with voltammetry. The two methods produce high quality data for thirty pollutant and biological trace elements. Results on archived specimens of human livers and intercomparisons of the two methods are reported.

Analyse des polychloro biphenyles, des hydrocarbures polycycliques aromatiques, et des pesticides dans les sediments marins, les tissus d'huitres, de moules et de poissons et dans le foie humain; ces echantillons font partie d'un lot de specimen qui ont ete stockes depuis 10 ans

A neutron activation analysis scheme based upon a radiochemical separation of the activation products has been developed. The method utilizes the inherent sensitivity of the activation reaction198Pt(n, γ)199Pt and counting of the daughter nuclide199Au. This nuclide is radiochemically separated from interfering activities by homogeneous precipitation as elemental gold. The remaining interference of the secondary reaction197Au(n,γ)198 Au(n,γ)199Au from gold in the samples is quantitatively assessed and corrected. During this process accurate gold concentrations in the samples are obtained at ultratrace levels. The analysis scheme is applied to gold and platinum determinations in biological Standard Reference Materials and human liver specimens. Gold and platinum are determined at concentrations of 5·10−11 g/g, and at higher levels.

A comprehensive approach to the analysis of human livers was developed in a pilot program for the National Environmental Specimen Bank that employed a combination of four analytical techniques. Refinements in this approach were needed for improvement in detection limits, more effective sample usage and to reduce the number of analytical steps that were involved. Since neutron activation analysis (NAA) had determined most of the elements, expansion of NAA was chosen to achieve these goals. Modifications in the instrumental NAA procedures, including the use of a Compton Suppressor System, gave increased sensitivity for some low level elements, such as arsenic and chromium. Radiochemical procedures that followed the instrumental counts increased the sensitivity for the elements chromium, selenium, arsenic, molybdenum, silver, antimony, and tin. Results are given for two radiochemical procedures that were applied following the modified procedure, either the use of an inorganic ion exchange column or a liquid/liquid extraction, and these are compared to instrumental results.

Using 201 foods from the United States Food and Drug Administration's Total Diet Study (FDA TDS), a mixed diet composite (USDIET-I) was prepared to represent the intake of 25-30-year-old males in the United States. Proximate analyses, phytate determination, and assays for nutrient elements and selected toxic elements, as well as organic nutrients were carried out on this composite. As part of a quality control exercise for a coordinated research program, atomic absorption spectrophotometry, inductively coupled atomic emission spectrometry, colorimetry and neutron activation analysis were used to determine up to 30 elements in this diet material. A comparison of the daily intakes of As, Ca, Cd, Cu, Fe, Hg, K, Mg, Mn, Na, P, Se and Zn from the composite USDIET-I shows excellent to good agreement with FDA TDS values calculated from results of single food analyses. These USDIET-I results demonstrate the feasibility of the mixed diet concept as a viable approach for a reliable assessment of daily intakes, especially for a number of elements such as Cd, Cr, Hg and Mo that occur at low concentrations in individual food products. Simultaneously, stability of some organic nutrients during storage was also investigated. Initial findings suggest that this program may also be useful in the development of reference materials for organic nutrients, for which there is a great need. These aspects are discussed.

Guided beams of cold neutrons being installed at a number of research reactors may become increasingly available for analytical research. A guided cold beam will provide higher neutron fluence rates and lower background interferences than in present facilities. In an optimized facility, fluence rates of 109 n·cm−2·s−1 are obtainable. Focusing a large area beam onto a small target will further increase the neutron intensity. In addition, the shift to lower neutron energy increases the effective cross sections. The absence of fast neutrons and gamma rays permits detectors to be placed near the sample without intolerable background, and thus the efficiency for counting prompt gamma rays can be much higher than in present systems. Measurements made at the hydrogen cold source of the FRJ-2 (DIDO) reactor at the KFA provide a numerical evaluation of the improvements in PGAA with respect to signal-to-background ratios of important elements and matrices.

Possible relationships between insufficient blood volume increases during pregnancy and infant mortality could be established with an adequate measurement procedure. An accurate and precise technique for blood volume measurements has been found in the isotope dilution technique using chromium-51 as a label for red blood cells. However, in a study involving pregnant women, only stable isotopes can be used for labeling. Stable chromium-50 can be determined in total blood samples before and after dilution experiments by neutron activation analysis (NAA) or mass spectrometry. However, both techniques may be affected by insufficient sensitivity and contamination problems at the inherently low natural chromium concentrations to be measured in the blood. NAA procedures involving irradiations with highly thermalized neutrons at a fluence rate of 2·1013 n·cm−2·s−1 and low background gamma spectrometry are applied to the analysis of total blood. Natural levels of chromium-50 in human and animal blood have been found to be

Chromium is one of the most difficult elements to accurately determine at the naturally occuring, ultratrace levels normally found in uncontaminated biological samples. In view of the importance of Cr, both as an essential and as a toxic element, efforts have focused on developing a simple, yet reliable, radiochemical procedure for Cr determination using neutron activation analysis. A number of problem areas have been identified in earlier methods, and an improved radiochemical separation procedure, based upon the liquid/liquid extraction of Cr(VI) into a solution of tribenzylamine/chloroform, has been developed. The fast neutron interference from Fe has been evaluated for the highly thermal RT-4 facility of the NBS Research Reactor, and Cr concentrations have been determined in samples of whole human blood collected under clean conditions and in two certified reference materials.