Study of provenance character on ancient porcelain of Yue Kiln at Silongkou with NAA

Chemical composition is an important information of studying the provenance character of ancient pottery and porcelain. The ancient celadon samples produced in Later Tang (850–907 A.D.) to Former Southern Song (1127–1279 A.D.) have been analyzed with NAA. Its provenance characteristic was compared with that of Hongzhou Kiln of Jiangxi Province and Yaozhou Kiln of Shanxi Province in this paper. The experimental data were studied with statistic methods. The results indicated that the chemical compositions of ancient porcelain body samples made in three kilns were different. The difference is able to be identified. The porcelain body materials of both Silongkou Yue Kiln and Hongzhou Kiln were similar. The samples of Yaozhou kiln in north of China existed obvious difference.     

Instrumental neutron activation analysis of prehistoric and ancient bone remains

Instrumental neutron activation analysis (INAA) was used to study the element contents in bones of prehistoric dinosaurs and bones of an ancient bear and an archantrop (ancient person), which were found on the territory of Uzbekistan. Concentrations of more than 25 elements were in the range of 0.043–3600 mg/kg. Multielement analyses of bone and soil samples were carried out by INAA using the WWR-SM research nuclear reactor. Results of measurements have shown that in the dinosaurs bones the concentration of the rare earth elements (REEs) were within 280–3200 mg/kg; the uranium content reached a very high value, up to 180 mg/kg, while in soils coating the dinosaurs bones this content was 4.2 mg/kg; in the bones of the archantrop it was 1.53 mg/kg and in the bones of a standard person its amount is less than 0.016 mg/kg.     

Determination of heavy metals in air conditioner dust using FAAS and INAA

The elements Cd, Cr, Cu, Mn, Ni, Pb and Zn were determined in dust samples collected from air conditioner (AC) filters from 15 commercial sites of Lahore using flame atomic absorption spectroscopy (FAAS). The elements Cr, Mn and Zn were also determined using instrumental neutron activation analysis (INAA). The results obtained showed that higher amounts of these metals were measured in these dust samples than normally found in soil. This was especially true for Cd, Cu, Pb and Zn. Generally the amounts of Cd, Cr and Mn did not vary throughout the city of Lahore but the amounts of the traffic related Cu, Pb and Zn elements had the more variable ranges of 30–140, 30–230 and 74–2810 mg/kg respectively. The concentrations obtained for Cr, Mn and Zn by INAA were found to be higher than those obtained using FAAS. Analysis of the data obtained showed the digestion procedure employed to be the possible cause for this occurrence. It was also found that Mn was being over-estimated by INAA due to the interference from the Mg peak.     

INAA laboratory results evaluation of inter-laboratory analysis test

Participation in inter-comparison programs is an important process to enhance the accuracy and precision of the analytical techniques. The Instrumental Neutron Activation Analysis laboratory (INAA) at Egypt Second Research Reactor (ETRR-2), ETRR-2 INAA Laboratory, was participated in three inter-comparison tests organized by AFRA Research Reactor Project for Socio-economic development. AFRAIV-12 Inter-laboratory Analysis Test 2007 is the third inter-laboratory analysis test within that project. The laboratories were asked to analyze for 43 essential and toxic elements using nuclear and related analytical techniques, with neutron activation analysis as the common technique. Five materials were distributed to the participants representing foodstuff, medicinal plants and aquatic biomonitors according to the focus of the AFRA IV-12 2006–2010 project. In this paper the ETRR-2 INAA Laboratory results is evaluated.     

Non-contact dilatometry of hard and soft porcelain compositions

Two different porcelain compositions were studied: a soft and a hard one. DTA, optical non-contact dilatometry and DSC were used to evaluate the thermal behaviour of the porcelain compositions with the aim to master the suitable thermal cycle for each. Results were interpreted on the basis of mineralogy and microstructure: the amorphous phase, abundant in soft porcelain, plays an important role on thermal expansion (8·10^–6 K^–1 for soft and 6·10^–6 K^–1 for hard at 1000°C). Thermal expansion behaviour as function of firing time was also studied. Non-contact dilatometry characterisation of porcelain bodies enable to master the suitable thermal cycle for the sintering.     

A compilation of X- and gamma-ray sensitivities from isotopes produced by the (n, γ) reaction for utilization in instrumental neutron activation analysis

A comprehensive compilation of X- and γ-ray emitting isotopes produced by the (n, γ) reaction is reported in this paper for application to instrumental neutron activation analysis (INAA). The X- and γ-ray sensitivities are computed theoretically by a computer code. Interfering photons from isotopes of neighbouring elements are identified by the code and the percentage interference is computed. Additionally an advantage factor (X-ray: γ-ray sensitivity) is computed, which is a figure of merit for X-ray spectroscopy in INAA. Further, mathematical representation of background continua for typical matrices encountered in INAA allow the calculation of elemental detection limits for the X-ray and γ-ray photons.     

Direct determination of trace rare earth elements in ancient porcelain samples with slurry sampling electrothermal vaporization inductively coupled plasma mass spectrometry

A method for the direct determination of trace rare earth elements in ancient porcelain samples by slurry sampling fluorinating electrothermal vaporization inductively coupled plasma mass spectrometry was developed with the use of polytetrafluoroethylene as fluorinating reagent. It was found that Si, as a main matrix element in ancient porcelain sample, could be mostly removed at the ashing temperature of 1200 °C without considerable losses of the analytes. However, the chemical composition of ancient porcelain sample is very complicated, which makes the influences resulting from other matrix elements not be ignored. Therefore, the matrix effect of ancient porcelain sample was also investigated, and it was found that the matrix effect is obvious when the matrix concentration was larger than 0.8 g l^− 1. The study results of particle size effect indicated that when the sample particle size was less than 0.057 mm, the particle size effect is negligible. Under the optimized operation conditions, the detection limits for rare earth elements by fluorinating electrothermal vaporization inductively coupled plasma mass spectrometry were 0.7 ng g^− 1 (Eu)–33.3 ng g^− 1(Nd) with the precisions of 4.1% (Yb)–10% (La) (c = 1 μg l^− 1, n = 9). The proposed method was used to directly determine the trace rare earth elements in ancient porcelain samples produced in different dynasty (Sui, Ming and Qing), and the analytical results are satisfactory.     

Metrological role of neutron activation analysis. IA. Inherent characteristics of relative INAA as a primary ratio method of measurement

In a series of three papers, the inherent characteristics of relative instrumental neutron activation analysis (INAA) as a primary ratio method of measurement, the unique functions of parametric INAA as an ideal back-up method of the relative INAA, and the valuable role of INAA in characterization of sampling behavior of individual elements in certified reference materials (CRMs) will be discussed. In this paper, the first of the series, the uncertainty evaluation and the traceability of values measured by neutron activation analysis (NAA), especially instrumental NAA (INAA), will be described to demonstrate the method at its ”the state-of-the-art” level can meet CCQM criteria for a primary ratio method. The scope and examples will be given. Received: 19 March 2001 Accepted: 2 October 2001     

Neutron activation techniques for the analysis of the soluble and particulate fractions of river water

Instrumental neutron activation analysis (INAA) techniques for filterable river water and suspended particulate matter (SPM) are described together with preconcentration techniques and simple radiochemical procedures to allow analyses when the trace element concentrations are very low (e.g. for mercury) and also when the sodium and calcium concentrations are very high. Detection limits are given for these methods and compared with those of other analytical techniques, including inductively coupled plasma emission spectrometry. The precision of measurement is between 10–15% for most elements and the detection limits are between 1 ng–1 μg.     

Effect of SnO<Subscript><Emphasis Type="Italic">x</Emphasis></Subscript> film on the bonding of titanium–porcelain

The SnO _x film was deposited on titanium by sol–gel dipping process. After drying at 80 °C for 5 h, the films were treated for 10 min at different temperature. A thin and coherent SnO _x film with small spherical pores obtained at 300 °C served as an effective oxygen diffusion barrier and improved titanium–porcelain adhesion. The SnO _x film changed the fracture mode of the titanium–porcelain system and improved the mechanical and chemical bonding between porcelain and titanium, resulted in the increased bonding strength of titanium–porcelain.     

Neutron activation analysis for identification of African mineral dust transport

A Gent stacked filter unit sampler was used to collect air particulate matter (APM) in separate coarse (PM_2.5–10) and fine (PM_2.5) size fractions, at a sub-urban site in Lisbon, Portugal. The sampling was done during the year 2001 and two daily samples were taken per week. The filters were analyzed for particulate mass by instrumental neutron activation analysis (INAA). The chemical analysis of APM levels and the study of the atmospheric dynamics by back-trajectories showed that most of the PM_2.5 and PM_2.5–10 peaks events were associated with air masses transport from the Saharan desert. High mineral load in ambient particulate matter levels were registered during the Saharan dust outbreaks. The accuracy of INAA to measure Fe, Sc and Sm was evaluated by NIST filter standards, revealing results with an agreement of ± 10%. This method constituted an important tool to identify these events.     

Instrumental neutron activation analysis of spherule samples recovered from the Pacific ocean sea sediment and Antarctic ice sheet

Chemical compositions of spherules separated from deep sea sediment dredged off Hawaiian islands and from Antarctic ice were measured by instrumental neutron activation analysis (INAA) using Kyoto University Reactor (KUR). Iron, cobalt, nickel, iridium, scandium and manganese contents in those spherules were determined to be 19.3–97.7%, 23–4370 mg·kg⁻¹, 0.08–7.04%, 0.84–35.4 mg·kg⁻¹, 1.4–44.3 mg·kg⁻¹ and 93.4 mg·kg⁻¹–7.2 %, respectively, and compared with each other. Particularly, iridium was detected in seven spherules among fourteen from Hawaii, but only one spherule among twenty-two from Antarctic, and those spherules turned out to be extraterrestrial in origin. However, it was shown that there was little difference in characteristics of elemental contents between both kinds of spherules, except for Ir-detected spherules.     

Determination of As by instrumental neutron activation analysis in sectioned hair samples for forensic purposes: chronic or acute poisoning?

Autopsy of 29-year old woman suspicious of committing suicide by the ingestion of As₂O₃ yielded contradictory findings. All pathological findings as well as clinical symptoms suggested acute poisoning, while a highly elevated As level of 26.4 μg g⁻¹ in her hair collected at the autopsy, which was determined with inductively coupled plasma mass spectrometry indicated chronic poisoning. To elucidate this discrepancy, instrumental neutron activation analysis (INAA) with proven accuracy was performed of another set of sectioned hair samples. Levels of As found by INAA in the range of 0.16–0.26 μg g⁻¹ excluded chronic poisoning, because the person died after approximately 14 h after the As₂O₃ ingestion. Two reasons for the discordant As results obtained by ICP-MS and INAA are considered: (1) accidental, non-removed contamination of hair on the As₂O₃ ingestion; (2) erroneous performance of ICP-MS.     

INAA for the determination of extractable organohalogens in precipitation in Shanghai, China

The paper presents the results of determination of extractable organohalogens (EOX) by instrumental neutron activation analysis (INAA), and polychlorinated biphenyls (PCBs) and organochlorine pesticides (OCPs) by gas chromatography (GC), in atmospheric precipitation in Shanghai, China, from January to August 2005. The results showed that EOCI was the major component of organohalogens in precipitation. A significant correlation between the concentrations of EOBr and EOI was observed (r ² = 0.75), which suggested that EOBr and EOI in precipitation might mainly come from the same sources. There were no clear seasonal trends for the concentrations of EOX. The concentrations of ΣPCBs ranged from 0.2–2.8 ng/l, with the dominant PCBs containing 3 to 5 chlorine atoms. HCH was the predominant pesticide in precipitation, accounting for over 80% of total OCPs, in which β-HCH took 28%–72% of total HCH. Also, there may be an evidence for significantly historical usage of DDT.     

Vanadium levels in marine organisms of Onagawa Bay in Japan

Vanadium in marine organisms from Onagawa Bay in Miyagi, Japan, was determined by an instrumental neutron activation analysis (INAA) method using anti-coincidence gamma-ray spectrometry at the Dalhousie University SLOWPOKE-2 Reactor (DUSR) facility in Canada. Seaweeds, cultivated oysters, plankton, and four different species of sea squirt were collected from Onagawa Bay during 2005–2008. Vanadium levels around 20 μg g⁻¹ (dry weight) were found in Japanese tangle and hijiki seaweeds. One species of sea squirt (Ciona savignyi) contained 160–500 ppm of V and it was highest among the four species of sea squirts studied. Protein-bound V species were separated by gel permeation chromatography (GPC) and the element determined by inductively coupled plasma atomic emission spectrometry (ICP-AES).     

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 the provenance of ancient Yaozhou celadon made at Lidipo and Shangdian during Kin period using nuclear technology

Yaozhou Kiln at Lidipo and Shangdian are two independent porcelain kiln groups of Yaozhou kiln series in Shanxi Province. Both of them were consisted of some individual porcelain kilns. The samples of 20 pieces of porcelain sherds produced in Shangdian and 43 pieces of porcelain sherds made in Lidipo sites which produced in Kin Dynasty (1115–1234 A.D.) have been collected. The main chemical compositions in body were determined by X-ray fluorescence (XRF). The contents of trace elements were measured using neutron activation analysis (NAA). Principal component analysis (PCA) and stepwise discriminant analysis were used to study the provenance characteristic of these samples. The results indicated that the main components and trace elements in the specimen can be used to reveal the provenance characteristic.     

Availability of essential trace elements in medicinal herbs used for diabetes mellitus and their possible correlations

Four plant parts (leaves, roots, fruits and seeds) of twenty samples of sixteen antidiabetic herbs including three commercially marketed capsules have been analyzed for 6 minor (Na, K, Ca, Cl, Mg, and P) and 21 trace (As, Ba, Br, Ce, Co, Cr, Cs, Cu, Eu, Fe, Hg, La, Mn, Rb, Sb, Sc, Se, Sm, Th, V and Zn) elements by instrumental neutron activation analysis (INAA). Further, Ni, Cd and Pb contents were determined by AAS. Elemental data were validated by simultaneously analyzing reference material (RM), MPH-2 Mixed Polish Herbs. Several elements such as Cr and V (1–2 μg/g), Rb (10–40 μg/g), Cs (80–300 ng/g), Se (∼100 ng/g) and Zn (25–60 μg/g) play an important role in diabetes mellitus. Interelemental linear correlations have been observed for Cu vs. Zn (r = 0.89) and Rb vs. Cs (r = 0.87). K/P ratio varies in a narrow range with a mean value of 6.2 ± 1.4. Toxic elements As and Hg were found in <1 μg/g whereas Cd and Pb were in ∼5 μg/g and <10 μg/g, respectively.     

Losses of elements in plant samples under the dry ashing process

Losses of trace elements in plant samples after dry ashing were investigated. Plant samples were heated in crucibles at 105–600°C for 0.5–24 hours in a muffle furnace. The amounts of elements remaining after heating were determined by INAA. The amounts of Cl and Br decreased over the range 200–400°C in all samples, especially in stem samples. The amount of Na increased over the range 450–600°C, possibly because of contamination from the crucibles. Dry ashing is suitable for analyzing most elements in plant samples.