A comparison between INAA and ICP-MS for the determination of element concentrations in marine sediments

In this study, instrumental neutron activation analysis (INAA) and inductively coupled plasma-mass spectrometry (ICP-MS) were used to compare results obtained by both techniques for sediment samples collected from the Patras Harbour, Western Greece. The accuracy of the methods was tested using reference materials. In total seven elements were measured by both techniques (Zn, Ni, Cr, Ba, As, U, Co). Results obtained by ICP-MS were compared with those obtained by INAA by applying paired t-test. Insignificant differences in mean concentration values were found for Zn, Ni, Cr and Ba, whereas the differences for As, Co and U were significant. Correlations between element concentrations measured by both techniques are also discussed.     

脱线柱预富集 ICP-MS法测定南极水样中的痕量元素

采用脱螯合阳离子树脂（D401）将待分析元素预富集并与基体元素分离，采用电感耦合等离子体质谱法（ICP－MS）测定了极拉斯曼丘陵地区环境水样中的难于或不能直接检测的超痕量元素Mn,Co,Ni,Cu,Cd,Ba和Pb；建立了一种准确，简便、快速的在线加内标准方法，被分析元素的测定灵敏度均提高了30倍左右；对于100mL，水样检测限为1．425ng/L-24.84ng/L。     

Use of INAA and PIXE for multipollutant air quality assessment and management

The objective of this paper was to assess the air pollution and the main sources of Air Particulate Matter in the Setúbal urban/industrial area, Portugal. PM_2.5 and PM_2.5?C10 were sampled in Nuclepore filters and lichens transplants were exposed during 9?months. The levels of elements in these two matrixes were measured by INAA and PIXE. A large data base was created and source apportionment was performed by using Principal Component Analysis. The results showed that the main sources of fine particles were anthropogenic and were related with traffic and local industry. There was an important contribution of natural sources, mainly for the coarse fraction, associated with the sea and the soil. Lichens characterization and mapping showed that different site-specific characteristics controlled the spatial distribution of different elements. This study showed that biomonitoring is an effective complementary method to traditional sampling systems.     

Characterization of Maya pottery by INAA and ICP-MS

A total of 81 pottery and 25 clay samples from the archaeological site and hinterland areas of Blue Creek in northwest Belize were analyzed by instrumental neutron activation analysis and inductively-coupled-plasma mass-spectrometry at the University of Missouri Research Reactor. Data generated for this study offers insight into local clay-resource variability and movement of pottery in the transition from Early (A.D. 250–600) to Late Classic (A.D. 600–850) occupation. Comparison of data generated by the two analytical techniques demonstrates the relative strengths and weaknesses of each method. This revised version was published online in July 2006 with corrections to the Cover Date.     

Assessment of ICP-MS for routine multielement analysis of soil samples in environmental trace element studies

Summary The suitability of inductively coupled plasma mass spectrometry (ICP-MS) following acid digestion of samples was evaluated for the routine determination of trace elements in contaminated and control soil samples. The contaminated samples were collected near an expressway and two secondary lead smelters in Toronto. All samples were acid digested in pressure vessels using a combination of reagents including hydrofluoric and perchloric acids. Consequently, the total amount of the elements (Pb, Sb, Cd, As, Mn, Mo and Cr) were being determined. In the case of lead direct comparison and isotope dilutional MS procedures were compared. Standard Reference Materials (SRM's) were run to allow an assessment of precision and accuracy. Isotope ratios were determined in the contaminated samples to evaluate whether this approach could be used, routinely, to determine the source of the lead. National Bureau of standards (NBS) 981 isotope ratio reference sample was used to evaluate the accuracy of the lead isotopic ratio data.Generally, the results obtained for the total amounts of the elements in the SRM's were in satisfactory agreement with the certified values. The measured isotopic ratios had a small positive bias compared to the NBS certified values. Isotope dilution MS values for Pb were superior in accuracy and precision to those obtained by direct comparison calibration. At the present state-of-the-art, routine isotope ratio measurements are not good enough for source typing in a study such as this. Values obtained in the present investigation compared well with those reported in a 1974 study of same areas.     

Variations in atmospheric trace element deposition studied by INAA of peat cores from ombrotrophic bogs

In the present work INAA is used to determine as many elements as possible in peat samples from ombrotrophic bogs. Results for depth distribution profiles of some elements of particular interest are presented for selected bogs from areas with highly different input from long-range atmospheric transport of pollutants. In addition to information on air pollution, the data provide knowledge about contribution from natural processes to the airborne supply of some elements, such as in the case of selenium.     

NAA and ICP-MS: A comparison between two methods for trace and ultra-trace element analysis

NAA and ICP-MS are both highly sensitive methods for multi-element trace-and ultra-trace element determination. A comparison between analytical figures of merit of both methods is made. Both methods have specific advantages that put them beyond competition for certain applications. It is concluded that ICP-MS can replace NAA for many routine analyses. NAA remains essential as a highly reliable and accurate reference method.     

INAA of trace impurities in aluminium clads

As a contribution to nondestructive neutron assay of reactor grade aluminium, a number of elements have been investigated qualitatively and quantiatively using a vertical channel in the IRT-5000 reactor with a thermal neutron flux of 7.6·10¹²n·cm^–2·s^–1. The -ray spectra of irradiated samples were analysed with a 30 cm³ Ge(Li) detector connected to an HP-computer and a 4096 channel analyser. The following impurities have been determined: Sc, Ca, Cr, Fe, Ni, Co, Zn, As, Sb, W, Au, Th and U, while Lu and Hf have been determined qualitatively only.     

Validation of methods for the determination of aluminium in fish gills by INAA and ICP-MS

In a European study of fish death in mixing zones of rivers with different acidities a reliable determination of Al and other elements in gills from freshwater fish was required, and both INAA and ICP-MS were studied as candidate reference methods. INAA requires minimum sample handling with a correspondingly small risk of contamination and no blank value; however, a careful study was needed of both nuclear interference from P and the increased detection limit caused by other major elements in the sample, before reliable results for Al could be ascertained. ICP-MS requires dissolution of the sample with a resulting risk of contamination and a significant reagent blank; while sensitivity was good, the interference from N created problems for sample decomposition in the microwave oven. Our experience with actual samples indicates that both methods suffer from considerable contamination problems, requiring that samples be handled in a clean bench with superpure reagents. Nuclear interference was determined experimentally by irradiating stoichiometric P-compounds with and without a Cd-shield; the observed interference of 1 g Al from 50 mg of P was found to require no correction in almost all cases. The accuracy of results was ascertained by analyzing SRM 1577 Bovine Liver.     

Determination of rare earth elements in rice by INAA and ICP-MS

In order to improve the accuracy of reactor neutron activation analysis, flux gradients and spectrum changes in the irradiation capsule have been studied at the Kyoto University Reactor (KUR). The flux and spectrum monitoring samples of Fe, Co, Au, Sb, U and Ni were placed at several positions in a polyethylene irradiation capsule of 24 mm inner diameter and 98 mm length, and were irradiated in a pneumatic irradiation facility (Pn-2). The flux gradients were found to be rather negligible in the vertical (axial) direction while they were considerable in the radial one. The flux gradient was around 5%/cm for thermal neutrons and 10%/cm for epithermal and fast neutrons. The spectrum changes were dependent on the materials (polyethylene and silica) filled in the capsule. Based on these observations, the effect of the flux gradients and spectrum changes on the accuracy of reactor neutron activation analysis was discussed.     

Toxic and trace element analysis of surface sediments from the Gulf of Saros by INAA and XRF methods

Some surface sediment samples, collected from 53 sampling sites of the Saros Gulf, were analyzed quantitatively by radioisotope energy dispersive X-ray fluorescence (EDXRF) and instrumental neutron activation analysis (INAA). Results indicated some correlations between Rb and Sr (r = 0.64), Fe₂O₃ and MnO (r = 0.59), Th and La (r = 0.71), Th and Ce (r = 0.64), Th and Sm (r = 0.60), concentration pairs. U and Th results are found to be compatible with those given in the literature for marine sediments.     

A comparison of INAA and ICP-MS/ICP-AES methods for the analysis of meteorite samples

Instrumental neutron activation analysis (INAA), inductively coupled plasma atomic emission spectrometry (ICP-AES) and ICP mass spectrometry (ICP-MS) (hereafter, ICPs) were applied to meteorite samples for the determination of elemental content. The analytical applicability and suitability of the three methods have been compared. Those comparisons led to the refinement of our analytical procedures for INAA and ICPs, yielding more reliable data. Our INAA data proved to be reliable enough for classifying meteorites, while the ICPs, especially ICP-MS, can characterize elemental abundance features in detail, as demonstrated by REE abundance patterns for the Allende meteorite. In this manner, INAA and ICPs can be used in a complementary fashion in cosmochemical studies.     

INAA and EDXRF applications in the age dynamics assessment of Zn content and distribution in the normal human prostate

An INAA, EDXRF and morphometric study was carried out to determine the zinc content and distribution in 87 prostates of health males aged from 5 days to 87 years. Also, an EDXRF method was used to determine zinc content in prostate fluid samples taken from 22 subjects aged 18 to 75. It was shown that intracellular zinc content increased highly in men over 40 years old. A hypothesis was suggested that excess of intracellular zinc might play an important role at both initiation and promotion stages of prostate carcinogenesis. This revised version was published online in July 2006 with corrections to the Cover Date.     

Development of a simple and fast ultrasound-assisted extraction method for trace element determination in tobacco samples using ICP-MS

The current study describes a simple and fast method for the determination of Ba, Cd, Co, Cr, Cu, Mn, Ni and Pb in tobacco samples. Commercial cigarettes obtained from local market stores were analysed by inductively coupled plasma mass spectrometry (ICP-MS) after ultrasound-assisted extraction in acidic medium, and the results were compared to those obtained following microwave-assisted digestion of the samples. The sonication time was evaluated from 0 to 60 min, and a 30 min extraction time was selected. The concentration of HNO₃ was also optimised at 0.7 mol L^?1. In order to verify the accuracy of the proposed method, a certified reference material was submitted to the same extraction protocol adopted for the samples, and good agreement with the certified values was obtained at a 95% confidence level, except for Co. The extraction of Pb was also semi-quantitative. A total of four tobacco samples were analysed, with concentrations ranging from 0.4 for Cr to 214.6 µg g^?1 for Mn. The proposed method was demonstrated to be fast, sensitive, precise and accurate for the determination of Ba, Cd, Cr, Cu, Mn an Ni and for the semi-quantitative analysis of Co and Pb in tobacco samples.     

Certification for trace elements and methyl mercury mass fractions in IAEA-456 marine sediment sample

Accreditation and Quality Assurance - Marine sediment certified reference material (CRM), IAEA-456 was recently produced by the Environment Laboratories of the International Atomic Energy Agency...     

INAA application in the assessment of Ag, Co, Cr, Fe, Hg, Rb, Sb, Sc, Se, and Zn mass fraction in pediatric and young adult prostate glands

The effect of age on trace element contents in intact prostate of 50 apparently healthy 0–30 year old males was investigated by neutron activation analysis with high resolution spectrometry of long-lived radionuclides. Mean values (M ± SΕΜ) for mass fraction (milligram per kilogram, on dry-weight basis) of trace elements were: Ag 0.0708 ± 0.0096, Co 0.0348 ± 0.0040, Cr 0.466 ± 0.069, Fe 100 ± 10, Hg 0.0258 ± 0.0025, Rb 12.6 ± 0.8, Sb 0.0576 ± 0.0066, Sc 0.0125 ± 0.0016, Se 0.478 ± 0.031, and Zn 273 ± 31, respectively. A strongly pronounced tendency of age-related increase in Se and Zn mass fraction and of age-related decrease in Co, Cr, Fe, and Sc mass fraction was observed in period of life from 0 to 30 years.     

Applications of mass spectrometry in the trace element analysis of biological materials

The importance of mass spectrometry for the analysis of biological material is illustrated by reviewing the different mass spectrometric methods applied and describing some typical applications published recently. Though atomic absorption spectrometry is used in the majority of analyses of biological material, most mass spectrometric methods have been used to some extent for trace element determination in biomedical research. The relative importance of the different methods is estimated by reviewing recent research papers. It is striking that especially inductively coupled plasma mass spectrometry is increasingly being applied, partly because the method can be used on-line after chromatographic separation, in speciation studies. Mass spectrometric methods prove to offer unique possibilities in stable isotope tracer studies and for this purpose also experimentally demanding methods such as thermal ionization mass spectrometry and accelerator mass spectrometry are frequently used.     

The role of different soil sample digestion methods on trace elements analysis: a comparison of ICP-MS and INAA measurement results

The measurement of trace-element concentration in soil, sediment and waste, is generally a combination of a digestion procedure for dissolution of elements and a subsequent measurement of the dissolved elements. “Partial” and “total” digestion methods can be used in environmental monitoring activities. To compare measurement results obtained by different methods, it is crucial to determine and to maintain control of the bias of the results obtained by these methods. In this paper, ICP-MS results obtained after matrix digestion with modified aqua regia (HCl+HNO₃+H₂O₂) method and two “total” digestion methods (microwave aqua regia+HF and HNO₃+HF) are compared with those obtained by instrumental neutron activation analysis, a non-destructive analytical method for the determination of the total mass concentrations of inorganic components in environmental matrices. The comparison was carried out on eight agricultural soil samples collected in one test area and measured by k₀-INAA and ICP-MS to determine As, Co, Cr, Sb and Zn mass concentration. The bias of results for As, Cd, Co, Cr, Cu, Ni, Pb, Sb and Zn of the three digestion methods were assessed using selected measurement standards. This paper highlights that the digestion procedure is an integral part of the measurement and can affect the measurement result in environmental analysis.