Homogeneity test of Chinese Biological Standard Reference Material by means of instrumental neutron activation analysis

A homogeneity test of 14 elements (Al, Cl, Mn, K, Ca, Ce, Th, Hf, Cs, Sc, Fe, Zn, Co and Eu) was made in Chinese Biological Standard Reference Material (peach leaves) by means of INAA. The procedures are described and the results are presented and discussed.     

Monostandard instrumental neutron activation analysis of Chinese Biological Standard Reference Material using short-lived radionuclides

A routine procedure for monostandard INAA using short-lived radionuclides with half-lives from 2 min to 15 hrs is described. Ten elements (Al, Mg, Ti, V, Mn, Cl, Na, K. Br and Cu) are determined in Chinese Biological Standard Reference Material (peach leaves). The quality of analysis was checked by analyzing the U. S. NBS Standard Reference Materials SRM-1571 and SRM-1648.     

Multielement analysis of Chinese Environmental Reference Materials by instrumental neutron activation analysis

Instrumental neutron activation analysis (INAA) has been applied for the simultaneous determination of up to 33 elements including major, minor and trace elements in the environmental reference materials soil and coal fly ash from China. The procedure involves both short and long irradiations followed by the measurement of the gamma spectra with a Ge(Li) detector. The analytical results are presented and discussed.     

Multielement analysis of lichen by instrumental neutron activation analysis

Lichen (species Trypethelium Eluteriae) is analysed for different elements. Nondestructive instrumental neutron activation analysis is employed for the multielemental analysis. Gamma-ray spectrometry is used for the identification and quantitative estimation of elements. Concentrations of 24 elements are reported. Gamma-ray spectrum of the lichen irradiated for 16 hours, delayed for 10 days, and counted for 10 hours on a 50 cm³ coaxial Ge(Li) detector is given.     

Multielement analysis of food spices by instrumental neutron activation analysis

Twenty-four elements in six food spices were estimated by non-destructive instrumental neutron activation analysis. The problems in determining Cu were discussed.     

Multielement analysis by sequential instrumental and radiochemical neutron activation

We measured 37 elements in six USGS geological camples and one NBS biological orchard leaf (OL) sample, using sequential INAA and radiochemical group separation coupled with high resolution, high efficiency Ge(Li), and a Ge(Li) with anticoincidence shields. The elemental concentrations in these samples vary over three orders of magnitude. Our results agree very well with the reported values. The rare earth values in PCC-1 are 2–4 times lower than the reported values. Precise REE patterns are defined in USGS samples, which are characteristic of the total rock types. The REE pattern in OL is identical to the mineral apatite. In addition to the possibility that OL may be contaminated by local soil, it is also possible that the uptake of REE trace elements by plants from soil is perhaps dominated by accessory mineral such as apatite, or plants take up the REE from bulk soil in a preferential manner as a smooth function of the REE ionic radii.     

Multielement determination in water by instrumental neutron activation analysis

Instrumental neutron activation analysis /INAA/ technique has been applied to a water sample to determine the elemental concentrations. The sample was irradiated with a neutron flux of 1.2×10¹² n cm^–2 s^–1 for two different periods followed by counting at three different decay times, using two coaxial type high-resolution Ge/Li/ detectors. The dominant elements determined in the water sample are Ca, Cl, Na, Mg, and K present in ppm-level while Co, I, Mn, Sm, and Sb are present in smaller amounts, approximately on the average 0.01 ppm. Only traces of other elements such as the rare-earth elements, Ag, As, Ba, Cu, Cd, Fe, Sr, W, Zn, seem to be present in the water sample.     

Multielement instrumental neutron activation analysis of silver-copper coins

Neutron activation, applied to silver and copper based coinage, leads to a measure of the mean concentrations of major and 12 trace elements, even if their distribution is heterogeneous. The drawbacks of this activation method applied to such a matrix are shielding effects and high radioactivity of major elements. Both effects were avoided by accurately calculating the correction coefficients and by choosing the optimal working conditions. Analytical results obtained lead to a better knowledge of the chronology and origin of Armorican protohistorical coinage.     

Multielement analysis of Nigerian chewing sticks by instrumental neutron activation analysis

In Nigeria, various parts of various species of native plants have long been used for dental hygiene, with reportedly considerable effectiveness. These materials are known as “chewing sticks”. This study was an effort to ascertain whether any unusual trace element concentrations might be present in Nigerian chewing sticks. Results are presented for 17 elements (Na, Mg, Al, Cl, K, Ca, Sc, V, Mn, Fe, Co, Zn, Br, Cs, La, Sm, Au) detected and measured in 12 species of such plants, via instrumental thermal-neutron activation analysis.     

Multielement determination in soil extracts by instrumental neutron activation analysis

Forest Swiss soils from 39 locations sampled ad three depths each were extracted with a buffered solution of pH 4.65 containing EDTA. Nearly 30 elements were determined by instrumental neutron activation analysis in these extracts. The results obtained are discussed in terms of efficiency of the extractant, precision and accuracy. Summariszed results are presented for the quantities fractions of the elements extracted.     

Multielement analysis of Northwestern Nigerian rocks by instrumental neutron activation analysis

Rock samples from seven different locations in northwestern Nigeria were analyzed by reactor instrumental neutron activation analysis and Ge(Li) gamma-ray spectrometry. Concentration values were obtained for 18 elements (As, Ce, Co, Cr, Cs, Eu, Fe, Hf, La, Lu, Sc, Sm, Sr, Ta, Tb, Th, U, Yb). The geochemical implications of the results are discussed.     

Multielement standards for instrumental neutron activation analysis of biological materials

Standards for instrumental neutron activation analysis (INAA) of biological materials are proposed. The standards are multielement solid solutions in phenol-formaldehyde resole resin (PFR) moulded as pellets weighing 30 to 50 mg. The concentrations of trace elements in the standards are selected so that, firstly, they are commensurable with their concentrations in the biological materials and, secondly, that the analytical lines of each of the elements incorporated in PFR are resolved with the aid of modern equipment. The principal standard contains 21 trace elements from among those of greatest interest for INAA of biological materials. This standard is recommended for work on high-resolution equipment. At the same time, standards of simpler trace element composition have been prepared and studied which can be used in work on simpler equipment or in solving particular problems in determination of certain groups of chemical elements.     

Multielement investigation of human bile by means of instrumental neutron activation analysis

In a study on gold containing antirheumatic agents, the portion of gold that was eliminated via liver was quantified. Seven patients whose gall bladders had just been removed surgically received 5 tablets RIDAURA^® containing a total amount of 4.35 mg gold in the chemical compound Auranofin. In the following 7 days samples of hepatic bile were collected and analyzed by instrumental neutron activation analysis (INAA). After a 3-day irradiation with neutrons in the Research Reactor Geesthacht (FRG) and after a waiting time of 5–10 days, the limit of detection for gold was about 0.03 ng. The gold concentration in bile reached the maximum value (≈65 ng/ml) after about 16 hours and decreased with a biological half-life, first of 21 hours and later, in the end phase, of 6.5 days. Further elements were determined in the hepatic bile: Na, Ca, Fe, Co, Zn, Se, Br, Rb, Cs, Ba, Hg and sporadically K, Sc, Cr, Ni, Sb, La, Ce, Eu, Tb, Hf, Ta, Th. Some of these elements occurred in clusters. The blank values of the quartz ampoules and the precision, accuracy and limit of detection of these elements are given. The element concentrations found in bile are compared with those in plasma and classified after BRAUER.     

Multielement determination in cattle hair infested withBoophilus microplus by instrumental neutron activation analysis

Instrumental neutron activation analysis (INAA) was applied to estimate the concentrations of Ca, Co, Cr, Cu, Fe, K, Mg, Mo, Mn, Na, Se and Zn in hair samples from Holstein-Friesan male calves, which were infested withBoophilus microplus larvae and, also from healthy animals. These results were obtained in order to evaluate if is there a significant difference between the trace element concentrations in hair samples from infested and healthy animals.     

Multielement comparison of instrumental neutron activation analysis techniques using reference materials

Several instrumental neutron activation analysis techniques (parametric, comparative, and k_o-standardization) are evaluated using three reference materials. Each technique is applied to National Institute of Standards and Technology standard reference materials, SRM 1577a (Bovine Liver) and SRM 2704 (Buffalo River Sediment), and the United States Geological Survey standard BHVO-1 (Hawaiian Basalt Rock). Identical (but not optimum) irradiation, decay, and counting schemes are employed with each technique to provide a basis for comparison and to determine sensitivities in a routine irradiation scheme. Fifty-one elements are used in this comparison; however, several elements are not detected in the reference materials due to rigid analytical conditions (e.g., insufficient length of irradiation or activity for radioisotope of interest decaying below the lower limit of detection before counting interval). Most elements are normally distributed around certified or consensus values with a standard deviation of 10%. For some elements, discrepancies are observed and discussed. The accuracy, precision, and sensitivity of each technique are discussed by comparing the analytical results to consensus values for the Hawaiian Basalt Rock to demonstrate the diversity of multielement applications.     

Multielement characterization of silicon carbide powders by instrumental neutron activation analysis and ICP-atomic emission spectrometry

Summary Instrumental neutron activation analysis (INAA) and inductively coupled plasma atomic emission spectrometry (ICP-AES) have been optimized for application to a comprehensive analysis of silicon carbide powders. Via medium- and long-lived indicator radionuclides with half lives between 2.3 h (¹⁶⁵Dy) and 12.4 a (¹⁵²Eu), INAA can detect 55 elements. Analytical parameters and experimental modes are given with limits of detection obtained for a silicon carbide powder of typical purity grade. For the performance of ICP-AES, a wet-chemical decomposition procedure was optimized for sample portions of about 1 g using a mixture of high-purity conc. HF, HNO₃ and H₂SO₄ for digestion in autoclaves with a PTFE-liner. For all investigated elements, recoveries 98% were obtained. By scanning wavelength profiles, interference-free emission lines were found for 56 elements. By the combined performance of INAA and ICP-AES, 66 elements were assayed in the analysed silicon carbide powder. The limits of detection were below 0.01 g/g for 24 elements, they were between 0.01 and 0.1 g/g for 17 and between 0.1 and 1 g/g for 15 elements. The remaining 10 elements were detectable at levels >1 g/g. The comparison of results of these two methods as well as of results obtained by other laboratories shows that, for the most common impurities, a satisfactory degree of accuracy could be achieved.     

Multielement determinations in ground water ultrafiltrates using inductively coupled plasma mass spectrometry and monostandard neutron activation analysis

Twelve ultrafiltrates of two ground waters rich in humic substances (up to 97.8 mg CL^–1) and in salinity (up to: cations 44.3 meq L^–1, anions 44.9 meq L^–1) were investigated with ICP-MS and with NAA in parallel. With both techniques 22 elements were analysed in a wide concentration range (mg/L to ng/L). Ultrafiltration at pore sizes from 1000 nm down to 1 nm lowers the humic colloid content as well as the concentration of the colloidborne polyvalent cations. Carbon interferences were studied in detail using artificially prepared model waters. The detection limits of ICP-MS in the ultrafiltrates (0.01 g/L–10 g/L) and in pure analyte solutions (5 ng/L–600 ng/L) are compared with those of NAA for pure water analysis (0.004 ng/L–50 ng/L).Dedicated to Professor Dr. H. Schmidbaur on the occasion of his 60th birthday     

Epithermal neutron activation analysis using the monostandard method

A method is described for epithermal neutron activation analysis of 17 elements in granite rock samples using a single standard. Gold has been used as a single comparator due to its relatively high resonance integral value (I₀=400 barn). In addition, it is preferable to Co in order to obtain a large epithermal activation in a short irradiation. The method of calculation is simple and rapid and can be done using a small calculator. Epithermal activation is able to overcome the difficulty arising from changing irradiation position as well as increasing the number of determinable elements by eliminating the interference from undesired isotopes which have relatively high thermal cross section values (₀), when reactor neutron flux is used. The coupling of epithermal activation with the monostandard method has the advantage of using a small Cd-cover which overcomes most of the difficulties arising in the relative method with large volume cadmium filters.     

Trace element determination in high-purity aluminum clad samples by k 0-based internal monostandard instrumental neutron activation analysis

The k₀-based internal monostandard instrumental neutron activation analysis (IM-INAA) method was applied for quantification of trace impurities in seven high purity aluminum samples used as fuel cladding in a research reactor. Samples along with BCS CRM 182 (Si–Al alloy) were irradiated in high flux reactor neutrons for 10–15 h. In situ detection efficiency, needed in concentration calculation ratio by IM-INAA, was obtained using gamma rays of activation products produced in the samples. Elemental concentration ratios obtained with respect to Fe (used as internal monostandard) were converted to absolute concentrations by determining concentration of Fe by relative method of NAA. Concentrations of ten trace elements (Sc, Cr, Co, Zn, Ga, La, Ce, Sm, W and Hf) including major element Fe were determined in this work. The method used is non-destructive in nature and does not need multielement standards. Results of IM-INAA were compared with those obtained by relative method of INAA and inductively coupled plasma atomic emission spectrometry (ICP-AES). Details of methodologies and results obtained by all methods are discussed and compared in the paper.