Analytical characterization of alcohol-ethoxylate substances by instrumental separation techniques

The characterization of alcohol-ethoxylate substances is a significant challenge in analytical science. Their importance in industry and society makes it necessary to have methods for their rapid, reliable characterization and quantification. This overview highlights the instrumental separation techniques for their analysis - chromatographic (e.g., gas, liquid and supercritical fluid chromatography) and electrophoretic (e.g., capillary, gel, capillary zone, and non-aqueous capillary electrophoresis and micellar electrokinetic chromatography). We summarize and explain analytical parameters for their characterization. We include selected references and examples to show the appropriateness of instrumental separation techniques for the analytical characterization of alcohol-ethoxylate substances.     

Statistical evaluation of recorded knowledge in nuclear and other instrumental analytical techniques

Summary The main points addressed in this study are the following: Statistical distribution patterns of published literature on instrumental analytical techniques 1981–1984; structure of scientific literature and heuristics for identifying active specialties and emerging hot spot research areas in instrumental analytical techniques; growth and growth rates of the literature in some of the identified hot research areas; quality and quantity in instrumental analytical research output.

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Statistische Auswertung von Veröffentlichungen in nuklearen und anderen instrumentellen analytischen Techniken

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Presented at the IAEA Advisory Group Meeting on Comparison of Nuclear Analytical Methods with Competitive Methods, October 3–7, 1986, Oak Ridge, TN, USA     

Radiochemical analysis of radionuclides difficult to measure for waste characterization in decommissioning of nuclear facilities

Some radiochemical analytical methods for the determination of important beta-radionuclides for decommissioning are presented. An analytical method is briefly described, which is used for the determination of ³H and ¹⁴C in steel and aluminum by combustion using commercial oxidizer. A leaching method was developed for the determination of ³H in the contaminated silica gel. A simple distillation method is presented for the determination of ¹⁴C in heavy water and wastewater sample. A method developed for the simultaneous determination of ³H, ¹⁴C, ³⁶Cl, ⁵⁵Fe, ⁶³Ni, ⁴¹Ca and ¹²⁹I in concrete, graphite, aluminium, lead, and steel is presented. The developed methods have been successfully used to analyse various materials for characterization of the waste during the decommissioning of Danish nuclear reactors.     

Application of ICP-MS and HR-ICP-MS for the characterization of solutions generated from corrosion testing of spent nuclear fuel

Summary The corrosion behavior of spent nuclear fuels under simulated geologically unsaturated and oxidizing conditions are being studied by subjecting both unirradiated and irradiated nuclear fuels to dripping groundwater. Solutions and solid materials are periodically sampled and subsequently analyzed to determine concentrations of groundwater and fuel components in these materials to elucidate corrosion mechanisms. The analyses are performed primarily by inductively coupled plasma mass spectrometry (ICP-MS). For ICP-MS we use the method of internal standardization with direct external calibration with multi-elemental standards possessing natural isotopic abundances for the determination of concentrations groundwater components and indirect instrumental response calibration for the determination of fuel components. Additionally, we are utilizing high resolution inductively coupled plasma mass spectrometry (HR-ICP-MS) to enhance our ability to determine concentrations of low-solubility actinides at ultratrace concentrations.     

Application of advanced nuclear analytical techniques for the electrocatalyst's characterization: Paving the path for mechanistic investigations

As the application of electrocatalyst continues to expand, envisaging the hidden mechanisms occurring at various length scale affecting the catalytic efficiency became important. To enhance the stability of electrocatalyst and reduce the cost, it is of paramount importance to reveal the active site's dynamics (using in situ techniques for getting the real-time information) which directly affect the reactions such as oxygen evolution reaction, hydrogen evolution reaction, and so on. Since such reactions are crucial for many engineering and scientific applications, in situ characterization techniques are required, which could capture such reactions happening at a different length and time scale. This article analyzes the recent progress made in the field of electrocatalyst's characterization using in situ neutron techniques. The article also paves the future path and has delineated the future challenges involved in multiscale correlative techniques (e.g., neutron techniques in the combination of synchrotron or microscopic techniques) used for getting the multiscale (atomic to micrometer range) mechanistic information about the electrocatalyst's working and degradation.     

现代仪器分析技术在中药炮制机理研究中的应用

现代分析技术以仪器分析为主,大量先进的现代仪器分析技术已经较广泛地应用于中药炮制机理研究领域,对阐明中药炮制的机理,提高中药饮片的质量控制水平起了很大的推动作用.本文对多种现代仪器分析技术进行介绍,并对其在中药炮制机理研究中的应用现状作一综述.     

Fuel cycle and nuclear waste

Summary The effects of -irradiation and waste chemistry on the degradation of ethylenediaminetetraacetic acid (EDTA) in a simulant of an organic complexant mixed waste from the U.S. D.O.E’s Hanford Site have been studied. Re-identification of degradation products from an earlier radiolysis study and the results of a new chemo-degradation study indicate that glyoxylate and several chelator fragments, both nitrosated and un-nitrosated, are responsible for most of EDTA’s chemodynamics in the simulated waste.     

Application of nuclear analytical techniques for assessment of coastal impact

Marine sediments contain a record of past events and proved to be an interesting indicator matrix for this study. Instrumental neutron activation analysis and energy dispersive X-ray fluorescence techniques offer adequate sensitivity for analysis of trace elements. Grain size analysis of sediment samples before and after tsunami showed a shift in textural characteristics of the sediment which is not observed during regular monsoon and seasonal changes. Some general characteristics of sediments revealed sand content ranges between 39 and 65% and silt from 33 to 53%. Clay content was found low averaging 5.4% and varied from 2 to 13% (by weight). The concentration of Cu, Ni, Fe, Pb, Zn, Mn, Rb, Sr, Ti, K, and Ca varies from 12 to 53, 19?C46, 21,952?C36,785, 21?C39, 39?C67, 335?C856, 47?C61, 223?C400, 4,991?C8,054, 11,000?C15,791, and 5,878?C11,214?mg?kg^?1, respectively. The positive correlation was observed for Cu, Ni, Ti, K, and Rb with respect to Fe. The negative correlation was observed for Ca, Sr, Zn, and Pb with respect to Fe, indicating the different source for these metals in the marine sediment. Decrease of the particle-reactive element in the tsunami impacted sediment indicates removal of clay component in the sediment, which is supported by the presence of low Th/U ratio.     

Non-destructive radioanalytical technique in characterization of anion exchangers Amberlite IRN78 and Indion H-IP

The present study deals with characterization of industrial grade anion exchange resins Amberlite IRN78 and Indion H-IP for which non-destructive radiotracer technique using ¹³¹I and ⁸²Br was used. The radioisotopes were used to trace the kinetics of iodide and bromide ion-isotopic exchange reactions taking place in the two resins. It was observed that under identical experimental conditions of 40.0 °C, 1.000 g of ion exchange resins and 0.003 M labeled iodide ion solution for iodide ion-isotopic exchange reaction, the values of specific reaction rate (min^?1), amount of iodide ion exchanged (mmol), initial rate of iodide ion exchange (mmol min^?1) and log K _d were 0.285, 0.544, 0.155 and 12.6 respectively for Amberlite IRN78 resin, which was higher than 0.093, 0.315, 0.029 and 4.9 respectively as that obtained by using Indion H-IP resins. Also at a constant temperature of 40.0 °C, as the concentration of labeled iodide ion solution increases 0.001–0.004 M, the percentage of iodide ions exchanged increases from 68.10 to 74.00 % for Amberlite IRN78 resin, which was higher than the increase of 40.20–42.80 % as observed for Indion H-IP resins. The identical trend was observed for the two resins during bromide ion-isotopic exchange reaction. The overall results indicate that that under identical experimental conditions Amberlite IRN78 resins shows superior performance over Indion H-IP resins.     

Quality assessment of hydrosphere in the vicinity of Czech nuclear power plants by radioanalytical methods

Summary The paper deals with the impact of nuclear plants and radioactive waste disposal on surface and ground water quality in their vicinity using various radiometric and radioanalytical methods. The impact of nuclear power plant Temelin on activation concentrations and fission products in hydrosphere, including tritium, was detected. The annual average tritium concentrations in Vltava River correspond to the previously calculated estimates for average and minimal quaranteed flow rates. The concentrations histories of ⁹⁰Sr and ¹³⁷Cs in surface water show a decreasing trend. This trend was not influenced by the nuclear power plant pilot operation. In the case of tritium, a concentration increase trend has been already observed since the startup of pilot operation. An attempt has made interpreting the sorption and diffusion data for radionuclides of cesium, strontium and tritium and technetium as representatives of multivalent elements. Sorption and diffusion data of ¹³⁷Cs and ⁹⁰Sr in contact with natural sorbent bentonite lead to the conclusion that both diffusion and batch sorption experiments can be simulated by an exchange model. Sorption of technetium on various bentonites plus additives materials is described. Retention of technetium on these solid phases is driven by sorption of reduced form of technetium Tc(IV).     

Equilibration studies of an inorganic ion exchange material with liquid nuclear waste simulant using radiotracer techniques

Ion exchange distribution coefficients of zirconium, ruthenium, europium, and strontium, elements found in high level nuclear waste, were determined for a new titanium hydrous oxide-type inorganic ion exchange compound. Coefficients were determined at ambient temperatures and at 85°C. The equilibrations were done in solutions simulating the composition of nuclear waste expected from the Allied-General Nuclear services, Barnwell. South Carolina plant. The progress of each reaction was monitored by adding a radiotracer of the element investigated to the simulated waste solution. Ambient temperature distribution coefficients ranging from a high of 1.2·10⁶ for Zr to a low of 58 for Eu were obtained when equal weights of ion exchange material were used. Significantly higher distribution coefficients were found at 85°C than at ambient temperatures. This work was supported by the U. S. Energy Research Development Administration.     

Application of instrumental neutron activation analysis to ceramic solid electrolytes

Beta" alumina isomorphs with different conducting cations were produced by ion exchange in molten salts. The concentration of the main component (Al), of conducting ions (Na⁺, Sr⁺⁺, Ba⁺⁺) and of chlorides from residues of the melt inside the exchanged material was determined by instrumental neutron activation analysis (INAA).Dedicated to Professor Günther Tölg on the occasion of his 60th birthday     

The contribution of nuclear activation techniques to medical science

Activation techniques have been used since their inception to analyse body fluids and tissues in medical research. In recent years they have also been adapted to analyse tissues in vivo. Their wider application is restricted by their complexity and relative inaccessibility, and inter-laboratory comparisons of analyses of reference materials continue to show serious discrepancies for some elements. Activation techniques contribute most to medical science when they are applied to important medical problems which cannot be solved in other ways and when they are used as reference techniques to evaluate simpler, more accessible methods.     

Automated radioanalytical determination of lead and beryllium

The automated modification of the radioanalytical determination of lead and beryllium using AutoAnalyzer modules has been developed. The method for lead determination is based on a two-phase isotope exchange of lead between the sample solution labelled with²¹²Pb and the standard lead diethyldithiocarbamate solution in carbon tetrachloride. For the determination of beryllium a substoichiometric isotope dilution method using⁷Be as tracer and acetylacetone in chloroform as extractant was used. As little as 0.02 μg/ml of lead and 2 μg/ml of beryllium can be determined by the methods above. The flow diagrams of the automated procedures are presented.     

Corrosion of simulated nuclear waste glass

Glasses are suitable host matrices for the immobilization of high-level radioactive wastes. The corrosion behaviour of nuclear waste glass in water is of considerable importance, since a potential route for returning of radionuclides to the biosphere is their leaching from the waste form into groundwater and subsequent transport by the groundwater to the surface. In this study, the preparation and characterization of borosilicate glasses of different chemical composition were investigated. Borosilicate glasses were doped with simulated nuclear waste oxides. The chemical corrosion in water of these glasses was followed by measuring the leach rates (g·cm^–2·day^–1), as a function of time. It was found that a simulated nuclear waste glass with the chemical composition (weight %), 15.61% Na₂O, 10.39% B₂O₃, 45.31% SiO₂, 13.42% ZnO, 6.61% TiO₂ and 8.66% waste oxides, is characterized by low melting temperature and with good corrosion resistance in water. Influence of passive layers on the leaching behaviour of nuclear waste glasses is discussed.     

Identification of selenoproteins in the endoplasmatic reticulum of the rat kidney by combination of radioanalytical techniques and biochemical methods

Investigations have been carried out on rats to obtain information about the selenium-containing proteins present in the microsomal fraction and especially in the endoplasmatic reticulum (ER) of the kidney. For the determination of the selenium levels instrumental neutron activation analysis via ⁷⁵Se was used. After labeling of rats in vivo with ⁷⁵Se-selenite and separation of the proteins in the renal homogenate and cell compartments by electrophoretic methods, the ⁷⁵Se-containing proteins were detected by autoradiography. In this way, six selenium-containing proteins with molecular masses of 15, 16, 20, 23-25, 40-42 and 58-60 were found in the endoplasmatic reticulum. All of those were characterized as selenocysteine-containing selenoproteins. This revised version was published online in August 2006 with corrections to the Cover Date.     

Chemical characterization of graphite by instrumental neutron activation analysis

Nuclear and commercial grade graphite samples were analysed by instrumental neutron activation analysis (INAA) using high flux reactor neutrons. Eleven elements (Na, K, As, Sc, Fe, Cr, Co, Zn, La, Ce, and Sm) were determined in eight samples of graphite (two nuclear grade and six commercial grade) by irradiating at a neutron flux of 3?×?10¹³ cm^?2 s^?1 in CIRUS reactor and assaying the activity by high-resolution gamma ray spectrometry using 40% relative efficiency HPGe detector coupled to an MCA. Concentrations of elements were determined by relative method of INAA. Results of both types of graphites as well as detection limits achieved by INAA method are discussed in the paper.     

A concomitant use of some radioanalytical and metallurgical methods: Application to the study of the thermal oxidation of titanium

Polycrystalline titanium samples were oxidized in pure oxygen under a 75 torr pressure, at temperatures ranging from 400°C to 500°C, and for times up to 2 hrs. A similar treatment was applied to some single crystal samples, so as to show the relationship between the crystallite orientation and the oxidation rate. The oxide films were studied by means of radioanalytical techniques, such as nuclear microanalysis, electron diffraction and ESCA, in addition to most classical techniques such as optical and electron microscopy. The complementary side of these methods is showed. They permit us to determine the contamination of the metallic surface introduced by the polishing treatments, the oxidation rate at constant temperature, and the structure of the oxides which exists in the films. These ones are especially TiO₂, Ti₃O₅, Ti₂O₃ and TiO.     

Application of the single comparator method to instrumental photon activation analysis

Journal of Radioanalytical and Nuclear Chemistry - Instrumental photon activation analysis (IPAA) is nondestructive and multi-elemental analysis method like instrumental neutron activation...     

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.