Analysis of pollutants in air and water using gas chromatography and headspace gas chromatography

Energy Technology Data Exchange (ETDEWEB)

Stenner, H.

1980-01-01

The combination 'personal sampling' with headspace gas chromatography to determine traces of formaldehyde, phenol and benzene in air is investigated in this work, with the aim of developing maximum workplace concentration values (MWL values). Further possible applications of gas chromatography in trace analysis in the environmentally protected area. The analysis of chromium in waste waters (Cr III as acetyl acetonate complex) is investigated as further possible application, whereby optimum conditions are obtained. A modified flame ionization detector was used to increase the detection sensitivity.

Microporous glasses for pro-ecological applications

International Nuclear Information System (INIS)

Procyk, B.; Stoch, L.; Kubacki, M.; Rewilak, M.; Soltysiak, J.

1994-01-01

Microporous glasses are obtained by appropriate thermal and chemical treatment. On account of their sorptive properties microporous glasses represent an excellent material for storing high-energy radioactive waste products in nuclear power engineering and for binding toxins in natural environment. Microporous glasses may be used as membranes non-organic, as gel filling in chromatography. They may find application in biochemistry, chemical, metallurgical, electrochemical and other industries. The above applications depend on the internal arrangement, size and shape of pores. (author). 4 refs, 4 figs, 1 tab

Changes in Wine Ethanol Content Due to Evaporation from Wine Glasses and Implications for Sensory Analysis.

Science.gov (United States)

Wollan, David; Pham, Duc-Truc; Wilkinson, Kerry Leigh

2016-10-12

The relative proportion of water and ethanol present in alcoholic beverages can significantly influence the perception of wine sensory attributes. This study therefore investigated changes in wine ethanol concentration due to evaporation from wine glasses. The ethanol content of commercial wines exposed to ambient conditions while in wine glasses was monitored over time. No change in wine ethanol content was observed where glasses were covered with plastic lids, but where glasses were not covered, evaporation had a significant impact on wine ethanol content, with losses from 0.9 to 1.9% alcohol by volume observed for wines that received direct exposure to airflow for 2 h. Evaporation also resulted in decreases in the concentration of some fermentation volatiles (determined by gas chromatography-mass spectrometry) and a perceptible change in wine aroma. The rate of ethanol loss was strongly influenced by exposure to airflow (i.e., from the laboratory air-conditioning unit), together with certain glass shape and wine parameters; glass headspace in particular. This is the first study to demonstrate the significant potential for ethanol evaporation from wine in wine glasses. Research findings have important implications for the technical evaluation of wine sensory properties; in particular, informal sensory trials and wine show judging, where the use of covers on wine glasses is not standard practice.

Ultra-high Performance Liquid Chromatography in Steroid Analysis

OpenAIRE

Salonen, Fanny

2017-01-01

The latest version of liquid chromatography is ultra-high performance (or pressure) chromatography (UHPLC). In the technique, short and narrow-bore columns with particle sizes below 3 µm are used. The extremely high pressure used results in very short analysis times, excellent separation, and good resolution. This makes UHPLC a good choice for steroidal analysis. Steroids are a highly interesting area of study; they can be recognized as biomarkers for several diseases and are a relevant topic...

Simultaneous analysis for water- and fat-soluble vitamins by a novel single chromatography technique unifying supercritical fluid chromatography and liquid chromatography.

Science.gov (United States)

Taguchi, Kaori; Fukusaki, Eiichiro; Bamba, Takeshi

2014-10-03

Chromatography techniques usually use a single state in the mobile phase, such as liquid, gas, or supercritical fluid. Chromatographers manage one of these techniques for their purpose but are sometimes required to use multiple methods, or even worse, multiple techniques when the target compounds have a wide range of chemical properties. To overcome this challenge, we developed a single method covering a diverse compound range by means of a "unified" chromatography which completely bridges supercritical fluid chromatography and liquid chromatography. In our method, the phase state was continuously changed in the following order; supercritical, subcritical and liquid. Moreover, the gradient of the mobile phase starting at almost 100% CO2 was replaced with 100% methanol at the end completely. As a result, this approach achieved further extension of the polarity range of the mobile phase in a single run, and successfully enabled the simultaneous analysis of fat- and water-soluble vitamins with a wide logP range of -2.11 to 10.12. Furthermore, the 17 vitamins were exceptionally separated in 4min. Our results indicated that the use of dense CO2 and the replacement of CO2 by methanol are practical approaches in unified chromatography covering diverse compounds. Additionally, this is a first report to apply the novel approach to unified chromatography, and can open another door for diverse compound analysis in a single chromatographic technique with single injection, single column and single system. Copyright © 2014. Published by Elsevier B.V.

Analysis of anabolic steroids in body fluids by capillary gas chromatography with a two-channel detection system and a computer.

Science.gov (United States)

Uralets, V P; Semenova, V A; Yakushin, M A; Semenov, V A

1983-11-25

A method is described for analysis of multi-component mixtures of steroid metabolites in biological fluids by means of capillary gas chromatography with glass and fused-silica columns and simultaneous detection of methoxylamine-trimethylsilyl derivatives with universal flame-ionization and selective nitrogen alkali flameionization detectors. A data system was applied to the on-line treatment of the results. Computer programs were designed for precise calculation of Kováts retention indices from the known values for selected natural urinary steroids. The programs allow the selection of nitrogen-containing components, normalized chromatogram plotting for both detection channels and qualitative and quantitative analysis. Results are presented on the detection of metabolites of methandrostenolone, 17 alpha-methyltestosterone, 19-nortestosterone and fluoxymesterone.

Plasma chromatography

International Nuclear Information System (INIS)

Anon.

1984-01-01

This book examines the fundamental theory and various applications of ion mobility spectroscopy. Plasma chromatography developed from research on the diffusion and mobility of ions. Topics considered include instrument design and description (e.g., performance, spectral interpretation, sample handling, mass spectrometry), the role of ion mobility in plasma chromatography (e.g., kinetic theory of ion transport), atmospheric pressure ionization (e.g., rate equations), the characterization of isomers by plasma chromatography (e.g., molecular ion characteristics, polynuclear aromatics), plasma chromatography as a gas chromatographic detection method (e.g., qualitative analysis, continuous mobility monitoring, quantitative analysis), the analysis of toxic vapors by plasma chromatography (e.g., plasma chromatograph calibration, instrument control and data processing), the analysis of semiconductor devices and microelectronic packages by plasma chromatography/mass spectroscopy (e.g., analysis of organic surface contaminants, analysis of water in sealed electronic packages), and instrument design and automation (hardware, software)

Elemental analysis of forensic glasses by inductively coupled plasma mass spectrometry

Science.gov (United States)

Almirall, Jose R.; Duckworth, Douglas C.; Bayne, Charles K.; Morton, Sherman A.; Smith, David H.; Koons, Robert D.; Furton, Kenneth G.

1999-02-01

Flat glass is a common type of evidence collected from the scenes of crimes such as burglaries, vandalism, and hit-and- run accidents. The usefulness of such evidence lies in the ability to associate the glass from the scene (or a suspect) to the original source. Physical and chemical analysis of the glass can be used for discrimination between the possible sources of glass. If the sample is large enough, physical attributes such as fracture matches, density, color, and thickness can be employed for comparison between a recovered fragment(s) to the suspect source. More commonly, refractive index (RI) comparisons are employed. Due to the improved control over glass manufacturing processes, RI values often cannot differentiate glasses where approximately 6 - 9% of casework samples are not expected to be distinguished by RI alone even if they originated from different sources. Employing methods such as NAA, XRF, ICP-AES, and ICP-MS for the comparison of trace elemental compositions has been shown to be more discriminating than RI comparisons. The multielement capability and the sensitivity of ICP-AES and ICP-MS provide for excellent discrimination power. In this work, the sources of variability in ICP-MS of glass analysis are investigated to determine possible sources of variation. The sources of variation examined include errors due to sample preparation, instrument accuracy and precision, and interlaboratory reproducibility. Other sources of variation include inhomogeneity across a sheet of glass from the same source. Analysis of variance has been applied to our ICP-MS analysis of NIST standards and to the interlaboratory comparisons of float glass samples collected across a sheet in a production facility. The results of these experiments allows for a more accurate interpretation of forensic glass data and a better understanding of the discriminating power (absolute and practical) of ICP-MS.

Analysis of Roman glass from Albania by PIXE–PIGE method

International Nuclear Information System (INIS)

Šmit, Ž.; Tartari, F.; Stamati, F.; Vevecka Priftaj, A.; Istenič, J.

2013-01-01

A series of 31 Roman glasses dated to the 1st–4th c. AD from the present Albania was analyzed by the combined PIXE–PIGE method. The analysis shows typical natron-based glass of the Roman period, though statistical treatment using principal component analysis and bivariate plots reveals four distinct groups, which are qualified by increased levels of potassium, magnesium and titanium–manganese–iron oxides, respectively. MgO content may exceed 2% and reach the level commonly accepted for halophytic plant-ash glass. The groups are formed on account of mineral impurities in the sand, which gives support to the thesis of multiple production centers of raw glass in the imperial age

Structural analysis and thermal behavior of diopside-fluorapatite-wollastonite-based glasses and glass-ceramics.

Science.gov (United States)

Kansal, Ishu; Tulyaganov, Dilshat U; Goel, Ashutosh; Pascual, Maria J; Ferreira, José M F

2010-11-01

Glass-ceramics in the diopside (CaMgSi2O6)-fluorapatite (Ca5(PO4)3F)-wollastonite (CaSiO3) system are potential candidates for restorative dental and bone implant materials. The present study describes the influence of varying SiO2/CaO and CaF2/P2O5 molar ratio on the structure and thermal behavior of glass compositions in the CaO-MgO-SiO2-P2O5-Na2O-CaF2 system. The structural features and properties of the glasses were investigated by nuclear magnetic resonance (NMR), infrared spectroscopy, density measurements and dilatometry. Sintering and crystallization behavior of the glass powders were studied by hot-stage microscopy and differential thermal analysis, respectively. The microstructure and crystalline phase assemblage in the sintered glass powder compacts were studied under non-isothermal heating conditions at 825 °C. X-ray diffraction studies combined with the Rietveld-reference intensity ratio (R.I.R) method were employed to quantify the amount of amorphous and crystalline phases in the glass-ceramics, while scanning electron microscopy was used to shed some light on the microstructure of resultant glass-ceramics. An increase in CaO/SiO2 ratio degraded the sinterability of the glass powder compacts, resulting in the formation of akermanite as the major crystalline phase. On the other hand, an increase in P2O5/CaF2 ratio improved the sintering behavior of the glass-ceramics, while varying the amount of crystalline phases, i.e. diopside, fluorapatite and wollastonite. Copyright © 2010. Published by Elsevier Ltd.

Analysis of early medieval glass beads - Glass in the transition period

Energy Technology Data Exchange (ETDEWEB)

Smit, Ziga, E-mail: ziga.smit@ijs.si [Faculty of Mathematics and Physics, University of Ljubljana, Jadranska 19, SI-1000 Ljubljana (Slovenia); Jozef Stefan Institute, Jamova 39, P.O.B. 3000, SI-1001 Ljubljana (Slovenia); Knific, Timotej [National Museum of Slovenia, Presernova 20, SI-1000 Ljubljana (Slovenia); Jezersek, David [Jozef Stefan Institute, Jamova 39, P.O.B. 3000, SI-1001 Ljubljana (Slovenia); Istenic, Janka [National Museum of Slovenia, Presernova 20, SI-1000 Ljubljana (Slovenia)

2012-05-01

Glass beads from graves excavated in Slovenia and dated archaeologically to the 7th-10th century AD were analysed by the combined PIXE-PIGE method. The results indicate two groups of glass; natron glass made in the Roman tradition and glass made with alkalis from the ash of halophytic plants, which gradually replaced natron glass after c. 800 AD. The alkalis used in the second group of glass seem to be in close relation to a variant of the Venetian white glass that appeared several centuries later. The origin of this glass may be traced to glass production in Mesopotamia and around the Aral Sea. All the mosaic beads with eye decoration, as well as most of the drawn-segmented and drawn-cut beads analysed, are of plant-ash glass, which confirms their supposed oriental origin.

Trends in the analysis of natural gas by capillary gas chromatography

NARCIS (Netherlands)

Cramers, C.A.M.G.; Rossum, van G.J.

1986-01-01

The importance of correct determination of physical and chemical properties of natural gas is evident. The calculation of calorific value or hydrocarbon dew point requires detailed analysis as can be provided by gas chromatography. Analysis by gas chromatography is a necessary complement to direct

Gas Chromatography-Mass Spectrometric Analysis and Insecticidal ...

African Journals Online (AJOL)

HP

Original Research Article. Gas Chromatography-Mass Spectrometric Analysis and ... into a natural fumigant/insecticide for the control of stored product insects. Keywords: Mallotus ..... stability as well as reduce cost. ACKNOWLEDGEMENT.

Kinetics of Cold-Cap Reactions for Vitrification of Nuclear Waste Glass Based on Simultaneous Differential Scanning Calorimetry - Thermogravimetry (DSC-TGA) and Evolved Gas Analysis (EGA)

Energy Technology Data Exchange (ETDEWEB)

Rodriguez, Carmen P.; Pierce, David A.; Schweiger, Michael J.; Kruger, Albert A.; Chun, Jaehun; Hrma, Pavel R.

2013-12-03

For vitrifying nuclear waste glass, the feed, a mixture of waste with glass-forming and modifying additives, is charged onto the cold cap that covers 90-100% of the melt surface. The cold cap consists of a layer of reacting molten glass floating on the surface of the melt in an all-electric, continuous glass melter. As the feed moves through the cold cap, it undergoes chemical reactions and phase transitions through which it is converted to molten glass that moves from the cold cap into the melt pool. The process involves a series of reactions that generate multiple gases and subsequent mass loss and foaming significantly influence the mass and heat transfers. The rate of glass melting, which is greatly influenced by mass and heat transfers, affects the vitrification process and the efficiency of the immobilization of nuclear waste. We studied the cold-cap reactions of a representative waste glass feed using both the simultaneous differential scanning calorimetry thermogravimetry (DSC-TGA) and the thermogravimetry coupled with gas chromatography-mass spectrometer (TGA-GC-MS) as complementary tools to perform evolved gas analysis (EGA). Analyses from DSC-TGA and EGA on the cold-cap reactions provide a key element for the development of an advanced cold-cap model. It also helps to formulate melter feeds for higher production rate.

Inert carriers for column extraction chromatography

International Nuclear Information System (INIS)

Katykhin, G.S.

1978-01-01

Inert carriers used in column extraction chromatography are reviewed. Such carriers are devided into two large groups: hydrophilic carriers which possess high surface energy and are well wetted only with strongly polar liquids (kieselguhrs, silica gels, glasses, cellulose, Al 2 O 3 ) and water-repellent carriers which possess low surface energy and are well wetted with various organic solvents (polyethylene, polytetrafluorethylene polytrifluorochlorethylene). Properties of various carriers are presented: structure, chemical and radiation stability, adsorption properties, extracting agent capacity. The effect of structure and sizes of particles on the efficiency of chromatography columns is considered. Ways of immovable phase deposition on the carrier and the latter's regeneration. Peculiarities of column packing for preparative and continuous chromatography are discussed

Contribution to high-temperature chromatography and high-temperature-gas-chromatography-mass spectrometry of lipids

International Nuclear Information System (INIS)

Aichholz, R.

1998-04-01

This thesis describes the use of high temperature gas chromatography for the investigation of unusual triacylglycerols, cyanolipids and bees waxes. The used glass capillary columns were pretreated and coated with tailor made synthesized high temperature stable polysiloxane phases. The selective separation properties of the individual columns were tested with a synthetic lipid mixture. Suitable derivatization procedures for the gaschromatographic analyses of neutral lipids, containing multiple bonds as well as hydroxy-, epoxy-, and carboxyl groups, were developed and optimized. Therefore conjugated olefinic-, conjugated olefinic-acetylenic-, hydroxy-, epoxy-, and conjugated olefinic keto triacylglycerols in miscellaneous plant seed oils as well as hydroxy monoesters, diesters and hydroxy diesters in bees waxes could be analysed directly with high temperature gas chromatography for the first time. In order to elucidate the structures of separated lipid compounds, high temperature gas chromatography was coupled to mass spectrometry and tandem mass spectrometry, respectively. Comparable analytical systems are hitherto not commercial available. Therefore instrumental prerequisites for a comprehensive and detailed analysis of seed oils and bees waxes were established. In GC/MS commonly two ionization methods are used, electron impact ionization and chemical ionization. For the analysis of lipids the first is of limited use only. Due to intensive fragmentation only weak molecular ions are observed. In contrast, the chemical ionization yields in better results. Dominant quasi molecular ions enable an unambiguous determination of the molecular weight. Moreover, characteristic fragment ions provide important indications of certain structural features of the examined compounds. Nevertheless, in some cases the chromatographic resolution was insufficient in order to separate all compounds present in natural lipid mixtures. Owing to the selected detection with mass spectrometry

Gas Chromatography-Mass Spectrometric Analysis of Nematicidal ...

African Journals Online (AJOL)

Gas Chromatography-Mass Spectrometric Analysis of Nematicidal Essential Oil of Valeriana ... Tropical Journal of Pharmaceutical Research ... have a potential to be developed to natural nematicides for the control of cereal cyst nematodes.

Durability Characteristics Analysis of Plastic Worm Wheel with Glass Fiber Reinforced Polyamide.

Science.gov (United States)

Kim, Gun-Hee; Lee, Jeong-Won; Seo, Tae-Il

2013-05-10

Plastic worm wheel is widely used in the vehicle manufacturing field because it is favorable for weight lightening, vibration and noise reduction, as well as corrosion resistance. However, it is very difficult for general plastics to secure the mechanical properties that are required for vehicle gears. If the plastic resin is reinforced by glass fiber in the fabrication process of plastic worm wheel, it is possible to achieve the mechanical properties of metallic material levels. In this study, the mechanical characteristic analysis of the glass-reinforced plastic worm wheel, according to the contents of glass fiber, is performed by analytic and experimental methods. In the case of the glass fiber-reinforced resin, the orientation and contents of glass fibers can influence the mechanical properties. For the characteristic prediction of plastic worm wheel, computer-aided engineering (CAE) analysis processes such as structural and injection molding analysis were executed with the polyamide resin reinforcement glass fiber (25 wt %, 50 wt %). The injection mold for fabricating the prototype plastic worm wheel was designed and made to reflect the CAE analysis results. Finally, the durability of prototype plastic worm wheel fabricated by the injection molding process was evaluated by the experimental method and the characteristics according to the glass fiber contents.

Impact of comprehensive two-dimensional gas chromatography with mass spectrometry on food analysis.

Science.gov (United States)

Tranchida, Peter Q; Purcaro, Giorgia; Maimone, Mariarosa; Mondello, Luigi

2016-01-01

Comprehensive two-dimensional gas chromatography with mass spectrometry has been on the separation-science scene for about 15 years. This three-dimensional method has made a great positive impact on various fields of research, and among these that related to food analysis is certainly at the forefront. The present critical review is based on the use of comprehensive two-dimensional gas chromatography with mass spectrometry in the untargeted (general qualitative profiling and fingerprinting) and targeted analysis of food volatiles; attention is focused not only on its potential in such applications, but also on how recent advances in comprehensive two-dimensional gas chromatography with mass spectrometry will potentially be important for food analysis. Additionally, emphasis is devoted to the many instances in which straightforward gas chromatography with mass spectrometry is a sufficiently-powerful analytical tool. Finally, possible future scenarios in the comprehensive two-dimensional gas chromatography with mass spectrometry food analysis field are discussed. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

PIXE analysis of western han dynasty ancient glasses unearthed in Yangzhou city

International Nuclear Information System (INIS)

Li Qinghui; Gu Donghong; Gan Fuxi; Zhang Bin; Ma Bo; Cheng Huansheng

2003-01-01

Chemical composition analysis is one of the most important research aspects to provide scientific proof for the technical origin and development of Chinese ancient glass. Proton induced X-ray emission (PIXE) technique is a kind of multi-element quantitative analysis method with high sensitivity and without destruction of samples. Chemical composition of the Western Han dynasty glass garment flakes, which were excavated from Yangzhou city, was analyzed by PIXE, quantitatively. It was found that these glass flakes were attributed to PbO-BaO-SiO 2 glass originated in China. These flakes all consist of a glass core and a corroded outer layer with different thickness. There are relatively higher PbO, P 2 O 5 and CaO, while much lower BaO and SiO 2 in the corroded layers than in the glass cores. The experimental results were discussed

Lipidomic analysis of biological samples: Comparison of liquid chromatography, supercritical fluid chromatography and direct infusion mass spectrometry methods.

Science.gov (United States)

Lísa, Miroslav; Cífková, Eva; Khalikova, Maria; Ovčačíková, Magdaléna; Holčapek, Michal

2017-11-24

Lipidomic analysis of biological samples in a clinical research represents challenging task for analytical methods given by the large number of samples and their extreme complexity. In this work, we compare direct infusion (DI) and chromatography - mass spectrometry (MS) lipidomic approaches represented by three analytical methods in terms of comprehensiveness, sample throughput, and validation results for the lipidomic analysis of biological samples represented by tumor tissue, surrounding normal tissue, plasma, and erythrocytes of kidney cancer patients. Methods are compared in one laboratory using the identical analytical protocol to ensure comparable conditions. Ultrahigh-performance liquid chromatography/MS (UHPLC/MS) method in hydrophilic interaction liquid chromatography mode and DI-MS method are used for this comparison as the most widely used methods for the lipidomic analysis together with ultrahigh-performance supercritical fluid chromatography/MS (UHPSFC/MS) method showing promising results in metabolomics analyses. The nontargeted analysis of pooled samples is performed using all tested methods and 610 lipid species within 23 lipid classes are identified. DI method provides the most comprehensive results due to identification of some polar lipid classes, which are not identified by UHPLC and UHPSFC methods. On the other hand, UHPSFC method provides an excellent sensitivity for less polar lipid classes and the highest sample throughput within 10min method time. The sample consumption of DI method is 125 times higher than for other methods, while only 40μL of organic solvent is used for one sample analysis compared to 3.5mL and 4.9mL in case of UHPLC and UHPSFC methods, respectively. Methods are validated for the quantitative lipidomic analysis of plasma samples with one internal standard for each lipid class. Results show applicability of all tested methods for the lipidomic analysis of biological samples depending on the analysis requirements

Advanced in the Forensic Analysis of Glass Fragments with a Focus on Refractive Index and Elemental Analysis.

Science.gov (United States)

Almirall, J R; Trejos, T

2006-07-01

Advances in technology provide forensic scientists with better tools to detect, to identify, and to individualize small amounts of trace evidence that have been left at a crime scene. The analysis of glass fragments can be useful in solving cases such as hit and run, burglaries, kidnappings, and bombings. The value of glass as "evidentiary material" lies in its inherent characteristics such as: (a) it is a fragile material that is often broken and hence commonly found in various types of crime scenes, (b) it can be easily transferred from the broken source to the scene, suspect, and/or victim, (c) it is relatively persistent, (d) it is chemically stable, and (e) it has measurable physical and chemical properties that can provide significant evidence of an association between the recovered glass fragments and the source of the broken glass. Forensic scientists have dedicated considerable effort to study and improve the detection and discrimination capabilities of analytical techniques in order to enhance the quality of information obtained from glass fragments. This article serves as a review of the developments in the application of both traditional and novel methods of glass analysis. The greatest progress has been made with respect to the incorporation of automated refractive index measurements and elemental analysis to the analytical scheme. Glass examiners have applied state-of-the-art technology including elemental analysis by sensitive methods such as ICPMS and LA-ICP-MS. A review of the literature regarding transfer, persistence, and interpretation of glass is also presented. Copyright © 2006 Central Police University.

Radiological analysis of plutonium glass batches with natural/enriched boron

International Nuclear Information System (INIS)

Rainisch, R.

2000-01-01

The disposition of surplus plutonium inventories by the US Department of Energy (DOE) includes the immobilization of certain plutonium materials in a borosilicate glass matrix, also referred to as vitrification. This paper addresses source terms of plutonium masses immobilized in a borosilicate glass matrix where the glass components include both natural boron and enriched boron. The calculated source terms pertain to neutron and gamma source strength (particles per second), and source spectrum changes. The calculated source terms corresponding to natural boron and enriched boron are compared to determine the benefits (decrease in radiation source terms) for to the use of enriched boron. The analysis of plutonium glass source terms shows that a large component of the neutron source terms is due to (a, n) reactions. The Americium-241 and plutonium present in the glass emit alpha particles (a). These alpha particles interact with low-Z nuclides like B-11, B-10, and O-17 in the glass to produce neutrons. The low-Z nuclides are referred to as target particles. The reference glass contains 9.4 wt percent B 2 O 3 . Boron-11 was found to strongly support the (a, n) reactions in the glass matrix. B-11 has a natural abundance of over 80 percent. The (a, n) reaction rates for B-10 are lower than for B-11 and the analysis shows that the plutonium glass neutron source terms can be reduced by artificially enriching natural boron with B-10. The natural abundance of B-10 is 19.9 percent. Boron enriched to 96-wt percent B-10 or above can be obtained commercially. Since lower source terms imply lower dose rates to radiation workers handling the plutonium glass materials, it is important to know the achievable decrease in source terms as a result of boron enrichment. Plutonium materials are normally handled in glove boxes with shielded glass windows and the work entails both extremity and whole-body exposures. Lowering the source terms of the plutonium batches will make the handling

Leachates analysis of glass from black and white and color televisions sets

Directory of Open Access Journals (Sweden)

Radovan Kukla

2012-01-01

Full Text Available The aim of work was to determine the content of selected elements in the glass from color and black and white television (TV sets. The amount of back taken TV sets in the Czech Republic increases annualy, which is associated with higher production of the waste glass. Currently there is 1.4 television sets for each household and the number of it should increase in future, because of higher standard of living and new technologies used. Waste glass treatment or landfilling may present, because of composition of the waste glass threat to the environment. One of the indicators of the polution from waste glass is leachate analysis, which can show us the content of hazardous substances in the waste glass, which can be released to the environment. A qualitative analysis of leachate samples was carried out by UV-VIS spectrophotometer. The results showed concentration of potencionaly hazardous substances contained in leachate samples. This was especially content of aluminum, cadmium, chromium, copper, molybdenum, nickel, lead, tin and zinc. Results of analyzes of the aqueous extract of glass were confronted with the limits specified in the currently valid legislation. Based on the results there is clear that in the case of landfilling of the glass from television sets, there is possibility of the contamination of landfill leachate by the elements, which are presented in the glass.

Glass Formation, Chemical Properties and Surface Analysis of Cu-Based Bulk Metallic Glasses

Directory of Open Access Journals (Sweden)

Akihisa Inoue

2011-04-01

Full Text Available This paper reviews the influence of alloying elements Mo, Nb, Ta and Ni on glass formation and corrosion resistance of Cu-based bulk metallic glasses (BMGs. In order to obtain basic knowledge for application to the industry, corrosion resistance of the Cu–Hf–Ti–(Mo, Nb, Ta, Ni and Cu–Zr–Ag–Al–(Nb bulk glassy alloy systems in various solutions are reported in this work. Moreover, X-ray photoelectron spectroscopy (XPS analysis is performed to clarify the surface-related chemical characteristics of the alloy before and after immersion in the solutions; this has lead to a better understanding of the correlation between the surface composition and the corrosion resistance.

Two-Dimensional Liquid Chromatography Analysis of Polystyrene/Polybutadiene Block Copolymers.

Science.gov (United States)

Lee, Sanghoon; Choi, Heejae; Chang, Taihyun; Staal, Bastiaan

2018-05-15

A detailed characterization of a commercial polystyrene/polybutadiene block copolymer material (Styrolux) was carried out using two-dimensional liquid chromatography (2D-LC). The Styrolux is prepared by statistical linking reaction of two different polystyrene- block-polybutadienyl anion precursors with a multivalent linking agent. Therefore, it is a mixture of a number of branched block copolymers different in molecular weight, composition, and chain architecture. While individual LC analysis, including size exclusion chromatography, interaction chromatography, or liquid chromatography at critical condition, is not good enough to resolve all the polymer species, 2D-LC separations coupling two chromatography methods were able to resolve all polymer species present in the sample; at least 13 block copolymer species and a homopolystyrene blended. Four different 2D-LC analyses combining a different pair of two LC methods provide their characteristic separation results. The separation characteristics of the 2D-LC separations are compared to elucidate the elution characteristics of the block copolymer species.

Application of gas chromatography to analysis of spirit-based alcoholic beverages.

Science.gov (United States)

Wiśniewska, Paulina; Śliwińska, Magdalena; Dymerski, Tomasz; Wardencki, Waldemar; Namieśnik, Jacek

2015-01-01

Spirit-based beverages are alcoholic drinks; their production processes are dependent on the type and origin of raw materials. The composition of this complex matrix is difficult to analyze, and scientists commonly choose gas chromatography techniques for this reason. With a wide selection of extraction methods and detectors it is possible to provide qualitative and quantitative analysis for many chemical compounds with various functional groups. This article describes different types of gas chromatography techniques and their most commonly used associated extraction techniques (e.g., LLE, SPME, SPE, SFE, and SBME) and detectors (MS, TOFMS, FID, ECD, NPD, AED, O or EPD). Additionally, brief characteristics of internationally popular spirit-based beverages and application of gas chromatography to the analysis of selected alcoholic drinks are presented.

Determination of boron in borosilicate glasses by neutron capture prompt gamma-ray activation analysis

Energy Technology Data Exchange (ETDEWEB)

Riley, Jr, J E; Lindstrom, R M

1987-01-01

Major levels of boron in borosilicate glasses were determined nondestructively by neutron activation analysis. The effects of neutron self-shielding by boron (1 to 8% by weight) are examined. Results of the analysis of a series of glasses with increasing boron composition are 1.150 +- .005% and 7.766 +- .035% for the low and high members of the series. Once analyzed, the glasses are useful as secondary standards for alpha track counting, and also ion and electron microprobe analyses of glasses. 12 refs.; 3 tables.

Group type analysis of asphalt by column liquid chromatography

Energy Technology Data Exchange (ETDEWEB)

Zhang, C.; Yang, J.; Xue, Y.; Li, Y. [Chinese Academy of Science, Taiyuan (China)

2008-07-01

An improved analysis method for characterization of asphalt was established. The method is based on column chromatography technique. The asphalts were separated into four groups: saturates, aromatics, resins, and asphaltenes, quantitatively. About 0.1 g of sample was required in each analysis. About 20 mL of n-heptanes was used to separate out saturates first. Then about 35 mL of n-heptanes/dichloromethane (.5, v/v) mixture was used to separate out aromatics. About 30 mL of dichloromethane/tetrahydrofuran (1/3, v/v) mixture was used to separate out resin. The quality of the separation was confirmed by infrared spectra (IR) and {sup 1}H NMR analysis. The model compounds, tetracosan for saturates, dibenz(o)anthracen for aromatics, and acetanilide for resins were used for verification. The IR and {sup 1}H NMR analysis of the prepared fractions from the column liquid chromatography were in good agreement that of pure reagents.

Potential application of gas chromatography to the analysis of hydrogen isotopes

International Nuclear Information System (INIS)

Warner, D.K.; Sprague, R.E.; Bohl, D.R.

1976-01-01

Gas chromatography is used at Mound Laboratory for the analysis of hydrogen isotopic impurities in gas mixtures. This instrumentation was used to study the applicability of the gas chromatography technique to the determination of the major components of hydrogen isotopic gas mixtures. The results of this study, including chromatograms and precision data, are presented

Comparison of gas chromatography/isotope ratio mass spectrometry and liquid chromatography/isotope ratio mass spectrometry for carbon stable-isotope analysis of carbohydrates

NARCIS (Netherlands)

Moerdijk-Poortvliet, Tanja C. W.; Schierbeek, Henk; Houtekamer, Marco; van Engeland, Tom; Derrien, Delphine; Stal, Lucas J.; Boschker, Henricus T. S.

2015-01-01

We compared gas chromatography/isotope ratio mass spectrometry (GC/IRMS) and liquid chromatography/isotope ratio mass spectrometry (LC/IRMS) for the measurement of δ(13)C values in carbohydrates. Contrary to GC/IRMS, no derivatisation is needed for LC/IRMS analysis of carbohydrates. Hence, although

Comparison of gas chromatography/isotope ratio mass spectrometry and liquid chromatography/isotope ratio mass spectrometry for carbon stable-isotope analysis of carbohydrates

NARCIS (Netherlands)

Moerdijk-Poortvliet, T.C.W.; Schierbeek, H.; Houtekamer, M.; van Engeland, T.; Derrien, D.; Stal, L.J.; Boschker, H.T.S.

2015-01-01

We compared gas chromatography/isotope ratio mass spectrometry (GC/IRMS) and liquid chromatography/isotope ratio mass spectrometry (LC/IRMS) for the measurement of d13C values in carbohydrates. Contrary to GC/IRMS, no derivatisation is needed for LC/IRMS analysis of carbohydrates. Hence, although

Comparison of gas chromatography/isotope ratio mass spectrometry and liquid chromatography/isotope ratio mass spectrometry for carbon stable-isotope analysis of carbohydrates

NARCIS (Netherlands)

Moerdijk-Poortvliet, T.C.W.; Schierbeek, H.; Houtekamer, M.; van Engeland, T.; Derrien, D.; Stal, L.J.; Boschker, H.T.S.

2015-01-01

Rationale: We compared gas chromatography/isotope ratio mass spectrometry (GC/IRMS) and liquid chromatography/isotope ratio mass spectrometry (LC/IRMS) for the measurement of δ13C values in carbohydrates. Contrary to GC/IRMS, no derivatisation is needed for LC/IRMS analysis of carbohydrates. Hence,

Glass sealing

Energy Technology Data Exchange (ETDEWEB)

Brow, R.K.; Kovacic, L.; Chambers, R.S. [Sandia National Labs., Albuquerque, NM (United States)

1996-04-01

Hernetic glass sealing technologies developed for weapons component applications can be utilized for the design and manufacture of fuel cells. Design and processing of of a seal are optimized through an integrated approach based on glass composition research, finite element analysis, and sealing process definition. Glass sealing procedures are selected to accommodate the limits imposed by glass composition and predicted calculations.

Colouration of medieval glass bracelets studied by total reflection x-ray fluorescence analysis

International Nuclear Information System (INIS)

Detcheva, Albena; Velinova, Ralitsa; Ivanova, Elisaveta; Jordanov, Juri; Karadjov, Metody

2014-01-01

The contents of 3d-transition metals (Ti, V, Cr, Mn, Fe, Co, Ni, Cu and Zn) in fragments of medieval glass bracelets, found in the necropolis of Stambolovo and the castle of Mezek, Bulgaria, were determined by total reflection X-ray fluorescence (TXRF) analysis using gallium as internal standard. The samples were analysed as slurries in Triton X 114. The experimental parameters: grain size of the glass sample, concentrations of glass sample, Triton X114 and internal standard in the slurry, volume of the slurry aliquot taken for analysis, as well as the excitation time, were optimised. For method validation the certified reference material BAM-S005 Type A soda-lime glass was used. It was proven that the elements Co, Mn and Fe are responsible for colour generation in the investigated glass samples. The precision of the determinations is characterised by an RSD in the range 3–11%

Analysis of some ancient glass samples unearthed in Sichuan area by PIXE

International Nuclear Information System (INIS)

Li Fei; Li Qinghui; Gan Fuxi

2007-01-01

Proton induced X-ray emission (PIXE) technique is an effective method for the chemical composition analysis of ancient glass samples without destruction. Chemical composition of the ancient glass samples dated from the Warring States Period (770-476 B.C.) to the Six Dynasties Period (220-589 A.D.), which were unearthed in Sichuan area, was quantitatively determined by the PIXE technique. The results show that the glass Bi (disc) and the glass eye beads of the Warring States Period all belong to the PbO-BaO-SiO 2 system. According to the composition and shape, we infer that these glass Bi and eye beads were made in China. Whereas, the chemical compositions of the glass ear pendants and beads of the Six Dynasties Period are varied, including K 2 O-CaO-SiO 2 , K 2 O-SiO 2 and other glass systems, Based on the obtained results and those from literatures, some questions related to the technical propagation of the ancient Chinese glass are discussed. (authors)

Principles of Micellar Electrokinetic Capillary Chromatography Applied in Pharmaceutical Analysis

Directory of Open Access Journals (Sweden)

Árpád Gyéresi

2013-02-01

Full Text Available Since its introduction capillary electrophoresis has shown great potential in areas where electrophoretic techniques have rarely been used before, including here the analysis of pharmaceutical substances. The large majority of pharmaceutical substances are neutral from electrophoretic point of view, consequently separations by the classic capillary zone electrophoresis; where separation is based on the differences between the own electrophoretic mobilities of the analytes; are hard to achieve. Micellar electrokinetic capillary chromatography, a hybrid method that combines chromatographic and electrophoretic separation principles, extends the applicability of capillary electrophoretic methods to neutral analytes. In micellar electrokinetic capillary chromatography, surfactants are added to the buffer solution in concentration above their critical micellar concentrations, consequently micelles are formed; micelles that undergo electrophoretic migration like any other charged particle. The separation is based on the differential partitioning of an analyte between the two-phase system: the mobile aqueous phase and micellar pseudostationary phase. The present paper aims to summarize the basic aspects regarding separation principles and practical applications of micellar electrokinetic capillary chromatography, with particular attention to those relevant in pharmaceutical analysis.

Application of micellar electrokinetic capillary chromatography for routine analysis of different materials

Directory of Open Access Journals (Sweden)

Injac Rade

2008-01-01

Full Text Available Micellar electrokinetic capillary chromatography (MEKC has become a popular mode among the several capillary electro-migration techniques. Most drug analysis can be performed by using MEKC because of its wide applicability. Separation of very complex mixtures, determination of drugs in the biological materials, etc., can be successfully achieved by MEKC. This review surveys typical applications of MEKC analysis. Recent advances in MEKC, especially with solid-phase extraction and large-volume sample stacking, are described. Modes of electrokinetic chromatography including MEKC, a separation theory of MEKC, environmental friendly analysis, and selectivity manipulation in MEKC are also briefly mentioned.

PIXE and ICP-AES analysis of early glass unearthed from Xinjiang (China)

Energy Technology Data Exchange (ETDEWEB)

Zhang, B. [Department of Technical Physics, School of Physics, Peking University, Beijing 100871 (China); Cheng, H.S. [Institute of Modern Physics, Fudan University, Shanghai 200433 (China)]. E-mail: hscheng@fudan.edu.cn; Ma, B. [School of Information Science and Engineering, Fudan University, Shanghai 200433 (China); Li, Q.H. [Shanghai Institute of Optics and Fine Mechanics, Chinese Academy of Sciences, Shanghai 201800 (China); Zhang, P. [Xinjiang Institute of Archaeology, Urumchi 830011 (China); Gan, F.X. [School of Information Science and Engineering, Fudan University, Shanghai 200433 (China); Shanghai Institute of Optics and Fine Mechanics, Chinese Academy of Sciences, Shanghai 201800 (China); Yang, F.J. [Institute of Modern Physics, Fudan University, Shanghai 200433 (China)

2005-10-15

Early glasses (about 1066 BC-220 AD) unearthed from Xinjiang of China were chemically characterized by using PIXE and ICP-AES. It was found that these glasses were basically attributed to PbO-BaO-SiO{sub 2} system, K{sub 2}O-SiO{sub 2} system, Na{sub 2}O-CaO-SiO{sub 2} system and Na{sub 2}O-CaO-PbO-SiO{sub 2} system. The results from the cluster analysis showed that some glasses had basically similar recipe and technology. The PbO-BaO-SiO{sub 2} glass and the K{sub 2}O-SiO{sub 2} glass were thought to come from the central area and the south of ancient China, respectively. The part of the Na{sub 2}O-CaO-SiO{sub 2} glass (including the Na{sub 2}O-CaO-PbO-SiO{sub 2} glass) might be imported from Mesopotamia, while the other part might be locally produced.

Methods for Measurement and Statistical Analysis of the Frangibility of Strengthened Glass

Directory of Open Access Journals (Sweden)

Zhongzhi eTang

2015-06-01

Full Text Available Chemically strengthened glass features a surface compression and a balancing central tension (CT in the interior of the glass. A greater CT is usually associated with a higher level of stored elastic energy in the glass. During a fracture event, release of a greater amount of stored energy can lead to frangibility, i.e., shorter crack branching distances, smaller fragment size, and ejection of small fragments from the glass. In this paper, the frangibility and fragmentation behaviors of a series of chemically strengthened glass samples are studied using two different manual testing methods and an automated tester. Both immediate and delayed fracture events were observed. A statistical method is proposed to determine the probability of frangible fracture for glasses ion exchanged under a specific set of conditions, and analysis is performed to understand the dependence of frangibility probability on sample thickness, CT, and testing method. We also propose a more rigorous set of criteria for qualifying frangibility.

The neutron activation analysis of archaeological glasses from Scandinavia and Britain

International Nuclear Information System (INIS)

Sanderson, D.C.W.; Hunter, J.R.

1982-01-01

Neutron Activation Analysis is used as a method of investigation into the technological development and raw materials used in the production of glass in the Ist millennium A.D. Samples were selected with two aims in mind: Firstly, there is the determination of whether or not vessel glass from thw two regions can be assigned to a common area of manufacture as has been suggested on the basis of major element analysis. Secondly, the results complement a project of major element analysis by the energy-dispersive X-ray fluorescence technique and can be used to provide a further characterisation of some raw materials by correlation with XRF data. The material analysed includes fragments from Helgoe, Sweden, and from Saxon Southamton (Hamwih). Samples and flux monitors were irradiated in the Herald reactor at Alkermaston for 48 hours and the gamma-ray spectra recorded in two counting periods, one week after irradiation and again after a further period of four weeks. A general discussion of the archaeological significance of the data is made together with a rview of problems that this technique presents with regard to the analysis of early glass. (author)

Analysis of short-chain acids from anaerobic bacteria by high-performance liquid chromatography.

OpenAIRE

Guerrant, G O; Lambert, M A; Moss, C W

1982-01-01

A standard mixture of 25 short-chain fatty acids was resolved by high-performance liquid chromatography, using an Aminex HPX-87 column. The acids produced in culture media by anaerobic bacteria were analyzed by high-performance liquid chromatography after extraction with ether and reextraction into a small volume of 0.1 N NaOH. The presence of fumaric acid in culture extracts of Peptostreptococcus anaerobius was confirmed by gas chromatography-mass spectrometry analysis of the trapped eluent ...

Simultaneous achiral-chiral analysis of pharmaceutical compounds using two-dimensional reversed phase liquid chromatography-supercritical fluid chromatography.

Science.gov (United States)

Venkatramani, C J; Al-Sayah, Mohammad; Li, Guannan; Goel, Meenakshi; Girotti, James; Zang, Lisa; Wigman, Larry; Yehl, Peter; Chetwyn, Nik

2016-02-01

A new interface was designed to enable the coupling of reversed phase liquid chromatography (RPLC) and supercritical fluid chromatography (SFC). This online two-dimensional chromatographic system utilizing RPLC in the first dimension and SFC in the second was developed to achieve simultaneous achiral and chiral analysis of pharmaceutical compounds. The interface consists of an eight-port, dual-position switching valve with small volume C-18 trapping columns. The peaks of interest eluting from the first RPLC dimension column were effectively focused as sharp concentration pulses on small volume C-18 trapping column/s and then injected onto the second dimension SFC column. The first dimension RPLC separation provides the achiral purity result, and the second dimension SFC separation provides the chiral purity result (enantiomeric excess). The results are quantitative enabling simultaneous achiral, chiral analysis of compounds. The interface design and proof of concept demonstration are presented. Additionally, comparative studies to conventional SFC and case studies of the applications of 2D LC-SFC in pharmaceutical analysis is presented. Copyright © 2015 Elsevier B.V. All rights reserved.

A Comparison of Protein Stability in Prefillable Syringes Made of Glass and Plastic.

Science.gov (United States)

Waxman, Lloyd; Vilivalam, Vinod D

2017-01-01

The development of protein therapeutics requires stabilization of these labile molecules during shipment and storage. Biologics, particularly monoclonal antibodies, are frequently packaged at high concentration in prefillable syringes traditionally made of glass. However, some biologics are unstable in glass due to sensitivity to silicone oil, tungsten, glue, or metal ions. Syringes made from the plastic cyclic olefin polymer, Daikyo Crystal Zenith® (CZ), with a Flurotec-laminated piston, have none of these issues. This study compared the stability of several proteins including biotherapeutics when stored up to 14 months at 5 °C and 25 °C in prefillable siliconized syringes made of glass or silicone oil-free CZ syringes, and when subjected to mild agitation by end-over-end rotation at room temperature. At each time point, proteins were analyzed by several techniques including turbidity, size exclusion high-performance liquid chromatography, reversed phase high-performance liquid chromatography, ion-exchange chromatography, electrophoresis, and light scattering to monitor changes in aggregation and degradation. The results show that proteins have comparable stability when stored in glass syringes or in syringes made of CZ sterilized by E-beam or autoclave. In addition, proteins stressed by agitation were generally more stable and aggregated less in syringes made of CZ than in ones made of glass. LAY ABSTRACT: Biotherapeutic protein drugs such as monoclonal antibodies are frequently packaged at high concentration in prefillable syringes, which allows the drug to be directly administered by the patient or caregiver. Protein drugs, or biologics, can be unstable, and may aggregate, particularly when shaken. These aggregates can be immunogenic, stimulating the body's immune system to produce antibodies that can reduce the drug's efficacy. Although prefillable syringes are traditionally made of glass, some biologics are unstable in glass syringes due to the presence of

Polymer Analysis by Liquid Chromatography/Electrospray Ionization Time-of-Flight Mass Spectrometry.

Science.gov (United States)

Nielen, M W; Buijtenhuijs, F A

1999-05-01

Hyphenation of liquid chromatography (LC) techniques with electrospray ionization (ESI) orthogonal acceleration time-of-flight (oa-TOF) mass spectrometry (MS) provides both MS-based structural information and LC-based quantitative data in polymer analysis. In one experimental setup, three different LC modes are interfaced with MS:  size-exclusion chromatography (SEC/MS), gradient polymer elution chromatography (GPEC/MS), and liquid chromatography at the critical point of adsorption (LCCC/MS). In SEC/MS, both absolute mass calibration of the SEC column based on the polymer itself and determination of monomers and end groups from the mass spectra are achieved. GPEC/MS shows detailed chemical heterogeneity of the polymer and the chemical composition distribution within oligomer groups. In LCCC/MS, the retention behavior is primarily governed by chemical heterogeneities, such as different end group functionalities, and quantitative end group calculations can be easily made. The potential of these methods and the benefit of time-of-flight analyzers in polymer analysis are discussed using SEC/MS of a polydisperse poly(methyl methacrylate) sample, GPEC/MS of dipropoxylated bisphenol A/adipic acid polyester resin, LCCC/MS of alkylated poly(ethylene glycol), and LCCC/MS of terephthalic acid/neopentyl glycol polyester resin.

Laser induced breakdown spectroscopy for analysis and characterization of degradation pathologies of Roman glasses

International Nuclear Information System (INIS)

Palomar, T.; Oujja, M.; García-Heras, M.; Villegas, M.A.; Castillejo, M.

2013-01-01

The feasibility and possibilities of laser induced breakdown spectroscopy (LIBS) in the full study of non-destructible historic glasses have been explored in the present work. Thirteen Roman glass samples, including seven entire glass beads, from the ancient town of Augusta Emerita (SW Spain) were characterized by LIBS in combination with other conventional techniques, such as scanning electron microscopy/energy dispersive X-ray spectrometry, X-ray fluorescence and ultraviolet–visible spectrophotometry. LIBS stratigraphic analysis, carried out by the application of successive laser pulses on the same spot, has been mainly targeted at characterizing particular features of non-destructible historic glasses, such as bulk chemical composition, surface degradation pathologies (dealkalinization layers and deposits), chromophores, and opacifying elements. The obtained data demonstrate that LIBS can be a useful and alternative technique for spectroscopic studies of historical glasses, especially for those conserved under burial conditions and when it deals with studying non-destructible samples. - Highlights: • Determination of chromophores and opacifiers in non-destructible glass by LIBS • Manganese is determined as principal component of dark deposits. • Antimony appears in all decorations while lead is only present in yellow ones. • Stratigraphic analysis enables the identification of dealkalinization layers

Laser induced breakdown spectroscopy for analysis and characterization of degradation pathologies of Roman glasses

Energy Technology Data Exchange (ETDEWEB)

Palomar, T. [Instituto de Historia, Centro de Ciencias Humanas y Sociales, CSIC, C/Albasanz 26-28, 28037 Madrid (Spain); Oujja, M., E-mail: m.oujja@iqfr.csic.es [Instituto de Química Física Rocasolano, CSIC, C/Serrano 119, 28006 Madrid (Spain); García-Heras, M.; Villegas, M.A. [Instituto de Historia, Centro de Ciencias Humanas y Sociales, CSIC, C/Albasanz 26-28, 28037 Madrid (Spain); Castillejo, M. [Instituto de Química Física Rocasolano, CSIC, C/Serrano 119, 28006 Madrid (Spain)

2013-09-01

The feasibility and possibilities of laser induced breakdown spectroscopy (LIBS) in the full study of non-destructible historic glasses have been explored in the present work. Thirteen Roman glass samples, including seven entire glass beads, from the ancient town of Augusta Emerita (SW Spain) were characterized by LIBS in combination with other conventional techniques, such as scanning electron microscopy/energy dispersive X-ray spectrometry, X-ray fluorescence and ultraviolet–visible spectrophotometry. LIBS stratigraphic analysis, carried out by the application of successive laser pulses on the same spot, has been mainly targeted at characterizing particular features of non-destructible historic glasses, such as bulk chemical composition, surface degradation pathologies (dealkalinization layers and deposits), chromophores, and opacifying elements. The obtained data demonstrate that LIBS can be a useful and alternative technique for spectroscopic studies of historical glasses, especially for those conserved under burial conditions and when it deals with studying non-destructible samples. - Highlights: • Determination of chromophores and opacifiers in non-destructible glass by LIBS • Manganese is determined as principal component of dark deposits. • Antimony appears in all decorations while lead is only present in yellow ones. • Stratigraphic analysis enables the identification of dealkalinization layers.

Analysis of leachants from strontium chlorapatite glass ceramics

International Nuclear Information System (INIS)

Vijayalakshmi, S.; Ushalakshmi, K.; Annapoorani, S.; Sriram, S.; Uma Maheshwari, R.; Deivanayaki, R.; Sekar, J.K.; Sankaran, K.

2013-01-01

Strontium chlorapatite glass ceramics is being tried out as one of the candidate matrices for immobilizing pyrochemical salt waste produced in the nuclear industry. To find-out the suitability of such material for immobilising the waste, leaching of various constituents of the ceramics in water is required. Therefore, in Chemistry Group of IGCAR experiments are being carried out with simulated salt waste (chlorides of Li, Na, K, Cs, Ba, Nd and Ce) of pyrochemical reprocessing method for studying the utilisation of strontium chlorapatite glass ceramics towards the immobilization of radioactive waste. Leaching behaviour study requires the determination of alkali, alkaline earth and rare earth elements in the leachant solutions of the glass ceramic material. Apart from cations, leaching study of anions especially chloride is required as the chloride salts are used in pyrochemical experiments. Considering the good sensitivity of alkali elements in Flame-AES method, all the alkali elements were determined by flame-AES. Ba, Sr and rare earth elements in the leachant solutions were determined using ICP-OES. Chloride was determined using ISE and IC. Standardisation of instrumental techniques and the application of various techniques for the sample analysis will be discussed in the paper. (author)

Strong Cation Exchange Chromatography in Analysis of Posttranslational Modifications: Innovations and Perspectives

Science.gov (United States)

Edelmann, Mariola J.

2011-01-01

Strong cation exchange (SCX) chromatography has been utilized as an excellent separation technique that can be combined with reversed-phase (RP) chromatography, which is frequently used in peptide mass spectrometry. Although SCX is valuable as the second component of such two-dimensional separation methods, its application goes far beyond efficient fractionation of complex peptide mixtures. Here I describe how SCX facilitates mapping of the protein posttranslational modifications (PTMs), specifically phosphorylation and N-terminal acetylation. The SCX chromatography has been mainly used for enrichment of these two PTMs, but it might also be beneficial for high-throughput analysis of other modifications that alter the net charge of a peptide. PMID:22174558

Microstructuring of glasses

CERN Document Server

Hülsenberg, Dagmar; Bismarck, Alexander

2008-01-01

As microstructured glass becomes increasingly important for microsystems technology, the main application fields include micro-fluidic systems, micro-analysis systems, sensors, micro-actuators and implants. And, because glass has quite distinct properties from silicon, PMMA and metals, applications exist where only glass devices meet the requirements. The main advantages of glass derive from its amorphous nature, the precondition for its - theoretically - direction-independent geometric structurability. Microstructuring of Glasses deals with the amorphous state, various glass compositions and their properties, the interactions between glasses and the electromagnetic waves used to modify it. Also treated in detail are methods for influencing the geometrical microstructure of glasses by mechanical, chemical, thermal, optical, and electrical treatment, and the methods and equipment required to produce actual microdevices.

Comment on 'Spherical 2+p spin-glass model: An analytically solvable model with a glass-to-glass transition'

International Nuclear Information System (INIS)

Krakoviack, V.

2007-01-01

Guided by old results on simple mode-coupling models displaying glass-glass transitions, we demonstrate, through a crude analysis of the solution with one step of replica symmetry breaking (1RSB) derived by Crisanti and Leuzzi for the spherical s+p mean-field spin glass [Phys. Rev. B 73, 014412 (2006)], that the phase behavior of these systems is not yet fully understood when s and p are well separated. First, there seems to be a possibility of glass-glass transition scenarios in these systems. Second, we find clear indications that the 1RSB solution cannot be correct in the full glassy phase. Therefore, while the proposed analysis is clearly naive and probably inexact, it definitely calls for a reassessment of the physics of these systems, with the promise of potentially interesting developments in the theory of disordered and complex systems

S-F graphic representation analysis of photoelectric facula focometer poroo-plate glass

Science.gov (United States)

Tong, Yilin; Han, Xuecai

2016-10-01

Optical system focal length is usually based on the magnification method with focal length measurement poroo-plate glass is used as base element measuring focal length of focometer. On the basis of using analysis of magnification method to measure the accuracy of optical lens focal length, an expression between the ruling span of poroo-plate glass and the focal length of measured optical system was deduced, an efficient method to work out S-F graph with AUTOCAD was developed, the selecting principle of focometer parameter was analyzed, and Applied examples for designing poroo-plate glass in S-F figure was obtained.

Hydrophilic interaction chromatography (HILIC) in the analysis of antibiotics.

Science.gov (United States)

Kahsay, Getu; Song, Huiying; Van Schepdael, Ann; Cabooter, Deirdre; Adams, Erwin

2014-01-01

This paper presents a general overview of the application of hydrophilic interaction chromatography (HILIC) in the analysis of antibiotics in different sample matrices including pharmaceutical, plasma, serum, fermentation broths, environmental water, animal origin, plant origin, etc. Specific applications of HILIC for analysis of aminoglycosides, β-lactams, tetracyclines and other antibiotics are reviewed. HILIC can be used as a valuable alternative LC mode for separating small polar compounds. Polar samples usually show good solubility in the mobile phase containing some water used in HILIC, which overcomes the drawbacks of the poor solubility often encountered in normal phase LC. HILIC is suitable for analyzing compounds in complex systems that elute near the void in reversed-phase chromatography. Ion-pair reagents are not required in HILIC which makes it convenient to couple with MS hence its increased popularity in recent years. In this review, the retention mechanism in HILIC is briefly discussed and a list of important applications is provided including main experimental conditions and a brief summary of the results. The references provide a comprehensive overview and insight into the application of HILIC in antibiotics analysis. Copyright © 2013 Elsevier B.V. All rights reserved.

Characterization and reactivity of sodium aluminoborosilicate glass fiber surfaces

Energy Technology Data Exchange (ETDEWEB)

Ortiz Rivera, Lymaris, E-mail: luo105@psu.edu [Materials Research Institute, Pennsylvania State University, University Park, PA 16802 (United States); Bakaev, Victor A.; Banerjee, Joy [Materials Research Institute, Pennsylvania State University, University Park, PA 16802 (United States); Mueller, Karl T. [Department of Chemistry, Pennsylvania State University, University Park, PA 16802 (United States); Pantano, Carlo G. [Materials Research Institute, Pennsylvania State University, University Park, PA 16802 (United States); Department of Materials Science and Engineering, Pennsylvania State University, University Park, PA 16802 (United States)

2016-05-01

Highlights: • XPS revealed that these fiber surfaces contain sodium carbonate weathering products. • IGC–MS data confirms the products of acetic acid reaction with sodium carbonate. • NMR data shows two closely spaced, but distinct sodium carboxylate peaks. • Acetic acid reacts with both sodium in the glass and sodium in the sodium carbonate. - Abstract: Multicomponent complex oxides, such as sodium aluminoborosilicate glass fibers, are important materials used for thermal insulation in buildings and homes. Although the surface properties of single oxides, such as silica, have been extensively studied, less is known about the distribution of reactive sites at the surface of multicomponent oxides. Here, we investigated the reactivity of sodium aluminoborosilicate glass fiber surfaces for better understanding of their interface chemistry and bonding with acrylic polymers. Acetic acid (with and without a {sup 13}C enrichment) was used as a probe representative of the carboxylic functional groups in many acrylic polymers and adhesives. Inverse gas chromatography coupled to a mass spectrometer (IGC–MS), and solid state nuclear magnetic resonance (NMR), were used to characterize the fiber surface reactions and surface chemical structure. In this way, we discovered that both sodium ions in the glass surface, as well as sodium carbonate salts that formed on the surface due to the intrinsic reactivity of this glass in humid air, are primary sites of interaction with the carboxylic acid. Surface analysis by X-ray photoelectron spectroscopy (XPS) confirmed the presence of sodium carbonates on these surfaces. Computer simulations of the interactions between the reactive sites on the glass fiber surface with acetic acid were performed to evaluate energetically favorable reactions. The adsorption reactions with sodium in the glass structure provide adhesive bonding sites, whereas the reaction with the sodium carbonate consumes the acid to form sodium-carboxylate, H

Analysis of glass from the post-Roman settlement Tonovcov grad (Slovenia) by PIXE–PIGE and LA-ICP-MS

Energy Technology Data Exchange (ETDEWEB)

Šmit, Ž., E-mail: ziga.smit@fmf.uni-lj.si [Faculty of Mathematics and Physics, University of Ljubljana, Jadranska 19, SI-1000 Ljubljana (Slovenia); Jožef Stefan Institute, Jamova 39, SI-1001 Ljubljana (Slovenia); Milavec, T. [Department of Archaeology, Faculty of Arts, University of Ljubljana, Zavetiška 5, SI-1000 Ljubljana (Slovenia); Fajfar, H. [Jožef Stefan Institute, Jamova 39, SI-1001 Ljubljana (Slovenia); Rehren, Th. [UCL Qatar, Education City, P.O. Box 23689, Doha (Qatar); Lankton, J.W. [UCL Institute of Archaeology, 31-34 Gordon Square, London WC1H 0PY (United Kingdom); Gratuze, B. [IRAMAT-Centre Ernest-Babelon, CNRS Université d’Orléans, 3D rue de la Ferollerie, 45071 Orléans Cedex 2 (France)

2013-09-15

The combined PIXE–PIGE method was used for the analysis of 43 glass fragments from the archaeological site Tonovcov grad in western Slovenia, with 10 of these additionally being analysed by LA-ICP-MS. The glass objects were attributed to the Late Antique production of the 4th–7th c. AD, with two examples of early Roman glass and three glass beads, one of them presumably of oriental origin. The analysis showed typical natron-type glass, produced in the Levantine region around the river Belus, and a few examples of HIMT glass, which could be recognized also in several other recycled objects. Only one glass bead, found in Early Medieval context, was made of the ash of halophytic plants.

Supercritical fluid chromatography hyphenated with twin comprehensive two-dimensional gas chromatography for ultimate analysis of middle distillates.

Science.gov (United States)

Adam, Frédérick; Thiébaut, Didier; Bertoncini, Fabrice; Courtiade, Marion; Hennion, Marie-Claire

2010-02-19

This paper reports the conditions of online hyphenation of supercritical fluid chromatography (SFC) with twin comprehensive two-dimensional gas chromatography (twin-GCxGC) for detailed characterization of middle distillates; this is essential for a better understanding of reactions involved in refining processes. In this configuration, saturated and unsaturated compounds that have been fractionated by SFC are transferred on two different GC x GC columns sets (twin-GCxGC) placed in the same GC oven. Cryogenic focusing is used for transfer of fractions into the first dimension columns before simultaneous GCxGC analysis of both saturated and unsaturated fractions. The benefits of SFC-twin-GC x GC are demonstrated for the extended alkane, iso-alkane, alkene, naphthenes and aromatics analysis (so-called PIONA analysis) of diesel samples which can be achieved in one single injection. For that purpose, saturated and unsaturated compounds have been separated by SFC using a silver loaded silica column prior to GC x GC analysis. Alkenes and naphthenes are quantitatively recovered in the unsaturated and saturated fractions, respectively, allowing their identification in various diesel samples. Thus, resolution between each class of compounds is significantly improved compared to a single GCxGC run, and for the first time, an extended PIONA analysis of diesel samples is presented. Copyright 2009 Elsevier B.V. All rights reserved.

Influence of Glass Property Restrictions on Hanford HLW Glass Volume

International Nuclear Information System (INIS)

Kim, Dong-Sang; Vienna, John D.

2001-01-01

A systematic evaluation of Hanford High-Level Waste (HLW) loading in alkali-alumino-borosilicate glasses was performed. The waste feed compositions used were obtained from current tank waste composition estimates, Hanford's baseline retrieval sequence, and pretreatment processes. The waste feeds were sorted into groups of like composition by cluster analysis. Glass composition optimization was performed on each cluster to meet property and composition constraints while maximizing waste loading. Glass properties were estimated using property models developed for Hanford HLW glasses. The impacts of many constraints on the volume of HLW glass to be produced at Hanford were evaluated. The liquidus temperature, melting temperature, chromium concentration, formation of multiple phases on cooling, and product consistency test response requirements for the glass were varied one- or many-at-a-time and the resultant glass volume was calculated. This study shows clearly that the allowance of crystalline phases in the glass melter can significantly decrease the volume of HLW glass to be produced at Hanford.

Advances in silver ion chromatography for the analysis of fatty acids and triacylglycerols-2001 to 2011.

Science.gov (United States)

Momchilova, Svetlana M; Nikolova-Damyanova, Boryana M

2012-01-01

An effort is made to critically present the achievements in silver ion chromatography during the last decade. Novelties in columns, mobile-phase compositions and detectors are described. Recent applications of silver ion chromatography in the analysis of fatty acids and triacylglycerols are presented while stressing novel analytical strategies or new objects. The tendencies in the application of the method in complementary ways with reversed-phase chromatography, chiral chromatography and, especially, mass detection are outlined.

A comparative finite elemental analysis of glass abutment supported and unsupported cantilever fixed partial denture.

Science.gov (United States)

Ramakrishaniah, Ravikumar; Al Kheraif, Abdulaziz A; Elsharawy, Mohamed A; Alsaleh, Ayman K; Ismail Mohamed, Karem M; Rehman, Ihtesham Ur

2015-05-01

The purpose of this study was to investigate and compare the load distribution and displacement of cantilever prostheses with and without glass abutment by three dimensional finite element analysis. Micro-computed tomography was used to study the relationship between the glass abutment and the ridge. The external surface of the maxilla was scanned, and a simplified finite element model was constructed. The ZX-27 glass abutment and the maxillary first and second premolars were created and modified. The solid model of the three-unit cantilever fixed partial denture was scanned, and the fitting surface was modified with reference to the created abutments using the 3D CAD system. The finite element analysis was completed in ANSYS. The fit and total gap volume between the glass abutment and dental model were determined by Skyscan 1173 high-energy spiral micro-CT scan. The results of the finite element analysis in this study showed that the cantilever prosthesis supported by the glass abutment demonstrated significantly less stress on the terminal abutment and overall deformation of the prosthesis under vertical and oblique load. Micro-computed tomography determined a gap volume of 6.74162 mm(3). By contacting the mucosa, glass abutments transfer some amount of masticatory load to the residual alveolar ridge, thereby preventing damage to the periodontal microstructures of the terminal abutment. The passive contact of the glass abutment with the mucosa not only preserves the health of the mucosa covering the ridge but also permits easy cleaning. It is possible to increase the success rate of cantilever FPDs by supporting the cantilevered pontic with glass abutments. Copyright © 2015 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Quantitative micro-Raman analysis of volcanic glasses: influence and correction of matrix effects

Science.gov (United States)

Di Muro, Andrea

2014-05-01

Micro-Raman spectroscopy, even though a very promising micro-analytical technique, is still not used to routinely quantify volatile elements dissolved in glasses. Following an original idea of Galeener and Mikkelsen (1981) for the quantification of hydroxyl (OH) in silica glass, several quantitative procedures have been recently proposed for the analysis of water, sulphur and carbon in natural glasses (obsidians, pumices, melt inclusions). The quantification of a single analyte requires the calibration of the correlation between the intensity I (height or area) of the related Raman band, normalized or not to a reference band RB, and the analyte concentration. For the analysis of alumino-silicate glasses, RB corresponds to one of the two main envelopes (LF and HF) related to the vibration of the glass network. Calibrations are linear, provided the increase in the analyte concentration does not dramatically affect RB intensity. Much attention has been paid to identify the most appropriate spectral treatment (spectra reduction; baseline subtraction; etc) to achieve accurate measurement of band intensities. I here show that the accuracy of Raman procedures for volatile quantification critically depends on the capability in predicting and in taking into account the influence of multiple matrix effects, which are often correlated with the average polymerization degree of the glass network. A general model has been developed to predict matrix effects affecting micro-Raman analysis of natural glasses. The specific and critical influence of iron redox state and pressure are discussed. The approach has been extensively validated for the study of melt inclusions and matrices spanning a broad range of compositions and dissolved volatile contents. References Analytical procedures Mercier, M, Di Muro, A., Métrich, N., Giordano, D., Belhadj, O., Mandeville, C.W. (2010) Spectroscopic analysis (FTIR, Raman) of water in mafic and intermediate glasses and glass inclusions

Analysis of the luminescent spectra of Eu{sup 3+} in glasses

Energy Technology Data Exchange (ETDEWEB)

Jiang, Sha; Wei, Xiantao; Chen, Zhejia; Chen, Yonghu, E-mail: yhuchen@ustc.edu.cn; Yin, Min

2013-11-15

The spectroscopy properties of lanthanide ions in glasses differ remarkably from crystal and powder samples due to superposition of transitions from many ions with different local environments. Eu{sup 3+} ions were doped in lead–borosilicate and boro–tellurite glass samples to probe the structural information and to reveal their effects on the luminescent properties of lanthanide ions. Three emission peaks were observed for {sup 5}D{sub 0}→{sup 7}F{sub 0} transition, with peak energies linearly dependent on the excitation wavelengths, and correlation between the intensity ratio of {sup 5}D{sub 0}→{sup 7}F{sub 0} versus {sup 5}D{sub 0}→{sup 7}F{sub 2} and the width of {sup 7}F{sub 1} was observed. The former indicates that there are three subsets of Eu{sup 3+} sites in the samples, with {sup 7}F{sub 0} being pushed downwards by {sup 7}F{sub J} (J=2, 4, and 6) by crystal-field J-mixing, and the latter can be quantitatively modeled by the adaptation of the theoretical model of Wen et al. [Phys. Chem. Chem. Phys. 12, 9933 (2010)] to account for the corrections due to the inhomogeneous broadening of {sup 7}F{sub J} (J=0, and1) crystal-field levels. The methods explored here can be applied to study other glass hosts for luminescent materials. -- Highlights: • The quantitative analysis of Eu{sup 3+5}D{sub 0}→{sup 7}F{sub 0} emission spectra in glasses. • Improved data fitting with the modified CF splitting width calculation method. • Demonstration of the generality of the spectral analysis method in two glasses.

EXAFS analysis of full color glasses and glass ceramics: local order and color

International Nuclear Information System (INIS)

Santa Cruz, Petrus A.; Sa, Gilberto F. de; Malta, Oscar L.; Silva, Jose expedito Cavalcante

1996-01-01

The generation and control of the relative intensities of the primary additive colors in solid state light emitters is very important to the development of higher resolution media, used in color monitors, solid state sensors, large area and flat displays and other optoelectronic devices. We have developed a multi-doped glassy material named FCG (full color glass, to generate and to control the primary light colors, allowing the simulation of any color of light by additive synthesis. Tm(III), Tb(III) and Eu(III) ions were used (0.01 to 5.0 mol%) as blue, green and red narrow emitters. A wide color gamut was obtained under ultraviolet excitation by varying the material composition. The chromaticity diagram is covered, including the white simulation. We proposed a mechanism to control the chromaticity of a fixed composition of the material, using the Er (III) as a selective quencher that may be deactivated by infrared excitation. Although this new material presents at this time a high efficiency, it may be improved because the energy transfer between the rare earth triad may be still reduced. Optical spectroscopy measurements confirms that it is still possible to improve the efficiency of the FCC material. EXAFS analysis will be used to probe the local environment around the triad of rare earth that generates the primary colors. For this purpose we have prepared single doped glasses with each component of the triad with the same concentration than FCG. The devitrification of these glasses will be analyzed in order to produce glassceramics with ion segregation. (author)

Association of glass fragments by their trace elemental content using ICP-MS and LA-ICP-MS in the analysis scheme

Science.gov (United States)

Almirall, Jose R.; Montero, Shirly; Furton, Kenneth G.

2002-08-01

The importance of glass as evidence of association between a crime event and a suspect has been recognized for some time. Glass is a fragile material that is often found at the scenes of crimes such as burglaries, hit-and-run accidents and violent crime offenses. The physical and chemical properties of glass can be used to differentiate between possible sources and as evidence of association between two fragments of glass thought to originate from the same source. Refractive index (RI) comparisons have been used for this purpose but due to the improved control over glass manufacturing processes, RI values often cannot differentiate glasses, even if the glass originates from different sources. Elemental analysis methods such as NAA, XRF, ICP-AES, and Inductively Coupled Plasma Mass Spectrometry (ICP-MS) have also been used for the comparison of trace elemental compositions and these techniques have been shown to provide an improvement in the discrimination of glass fragments over RI comparisons alone. The multi-element capability and the sensitivity of ICP-MS combined with the simplified sample introduction of laser ablation prior to ion detection provides for an excellent and relatively non-destructive technique for elemental analysis of glass fragments. The methodology for solution analysis (digestion procedure) and solid sample analysis (laser ablation) of glass is reported and the analytical results are compared. An isotope dilution method is also reported as a high precision technique for elemental analysis of glass fragments. The optimum sampling parameters for laser ablation, for semi-quantitative analysis and element ratio comparisons are also presented. Finally, the results of a case involving the breaking of 15 vehicle windows in an airport parking lot and the association of a suspect to the breakings by the glass fragments found on his person are also presented.

Direct uranium isotope ratio analysis of single micrometer-sized glass particles

OpenAIRE

Kappel, Stefanie; Boulyga, Sergei F.; Prohaska, Thomas

2012-01-01

We present the application of nanosecond laser ablation (LA) coupled to a ‘Nu Plasma HR’ multi collector inductively coupled plasma mass spectrometer (MC-ICP-MS) for the direct analysis of U isotope ratios in single, 10–20 μm-sized, U-doped glass particles. Method development included studies with respect to (1) external correction of the measured U isotope ratios in glass particles, (2) the applied laser ablation carrier gas (i.e. Ar versus He) and (3) the accurate determination of lower abu...

Use and practice of achiral and chiral supercritical fluid chromatography in pharmaceutical analysis and purification.

Science.gov (United States)

Lemasson, Elise; Bertin, Sophie; West, Caroline

2016-01-01

The interest of pharmaceutical companies for complementary high-performance chromatographic tools to assess a product's purity or enhance this purity is on the rise. The high-throughput capability and economic benefits of supercritical fluid chromatography, but also the "green" aspect of CO2 as the principal solvent, render supercritical fluid chromatography very attractive for a wide range of pharmaceutical applications. The recent reintroduction of new robust instruments dedicated to supercritical fluid chromatography and the progress in stationary phase technology have also greatly benefited supercritical fluid chromatography. Additionally, it was shown several times that supercritical fluid chromatography could be orthogonal to reversed-phase high-performance liquid chromatography and could efficiently compete with it. Supercritical fluid chromatography is an adequate tool for small molecules of pharmaceutical interest: synthetic intermediates, active pharmaceutical ingredients, impurities, or degradation products. In this review, we first discuss about general chromatographic conditions for supercritical fluid chromatography analysis to better suit compounds of pharmaceutical interest. We also discuss about the use of achiral and chiral supercritical fluid chromatography for analytical purposes and the recent applications in these areas. The use of preparative supercritical fluid chromatography by pharmaceutical companies is also covered. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

MEMS-Based Micro Gas Chromatography: Design, Fabrication and Characterization

OpenAIRE

Zareian-Jahromi, Mohammad Amin

2009-01-01

This work is focused on the design, fabrication and characterization of high performance MEMS-based micro gas chromatography columns having wide range of applications in the pharmaceutical industry, environmental monitoring, petroleum distillation, clinical chemistry, and food processing. The first part of this work describes different approaches to achieve high-performance microfabricated silicon-glass separation columns for micro gas chromatographic (µGC) systems. The capillary width effec...

Separation techniques: Chromatography

Science.gov (United States)

Coskun, Ozlem

2016-01-01

Chromatography is an important biophysical technique that enables the separation, identification, and purification of the components of a mixture for qualitative and quantitative analysis. Proteins can be purified based on characteristics such as size and shape, total charge, hydrophobic groups present on the surface, and binding capacity with the stationary phase. Four separation techniques based on molecular characteristics and interaction type use mechanisms of ion exchange, surface adsorption, partition, and size exclusion. Other chromatography techniques are based on the stationary bed, including column, thin layer, and paper chromatography. Column chromatography is one of the most common methods of protein purification. PMID:28058406

Multiresidue analysis of pesticides in olive oil by gel permeation chromatography followed by gas chromatography-tandem mass-spectrometric determination

International Nuclear Information System (INIS)

Sanchez, Andres Garcia; Martos, Natividad Ramos; Ballesteros, Evaristo

2006-01-01

A method for the multiresidue analysis of olive oil samples for 26 pesticides is proposed. Residual pesticides are extracted from oil using an n-hexane/acetonitrile mixture, extracts being cleaned-up by gel permeation chromatography (GPC) for analysis by gas chromatography-tandem mass spectrometry (GC-MS/MS). Electron ionization and chemical ionization are employed in a single analysis for the determination of pesticides. Pesticide recoveries from virgin and refined olive oil spiked with 10, 100 and 250 μg/kg concentrations of the pesticides ranged from 83.8 to 110.3%. The proposed method features good sensitivity: its limits of quantification are low enough to allow pesticide residues to be determined at concentrations below the maximum residue levels legally accepted. The precision, expressed as relative standard deviation, ranges from 4.93 to 8.11%. Applicability was tested on 40 olive oil samples. Several pesticides were detected in most of the virgin olive oil samples. By contrast, refined olive samples contained few pesticides, and only endosulfan sulphate was detected in all

Analysis of form deviation in non-isothermal glass molding

Science.gov (United States)

Kreilkamp, H.; Grunwald, T.; Dambon, O.; Klocke, F.

2018-02-01

Especially in the market of sensors, LED lighting and medical technologies, there is a growing demand for precise yet low-cost glass optics. This demand poses a major challenge for glass manufacturers who are confronted with the challenge arising from the trend towards ever-higher levels of precision combined with immense pressure on market prices. Since current manufacturing technologies especially grinding and polishing as well as Precision Glass Molding (PGM) are not able to achieve the desired production costs, glass manufacturers are looking for alternative technologies. Non-isothermal Glass Molding (NGM) has been shown to have a big potential for low-cost mass manufacturing of complex glass optics. However, the biggest drawback of this technology at the moment is the limited accuracy of the manufactured glass optics. This research is addressing the specific challenges of non-isothermal glass molding with respect to form deviation of molded glass optics. Based on empirical models, the influencing factors on form deviation in particular form accuracy, waviness and surface roughness will be discussed. A comparison with traditional isothermal glass molding processes (PGM) will point out the specific challenges of non-isothermal process conditions. Furthermore, the underlying physical principle leading to the formation of form deviations will be analyzed in detail with the help of numerical simulation. In this way, this research contributes to a better understanding of form deviations in non-isothermal glass molding and is an important step towards new applications demanding precise yet low-cost glass optics.

Forensic comparative glass analysis by laser-induced breakdown spectroscopy

International Nuclear Information System (INIS)

Bridge, Candice M.; Powell, Joseph; Steele, Katie L.; Sigman, Michael E.

2007-01-01

Glass samples of four types commonly encountered in forensic examinations have been analyzed by laser-induced breakdown spectroscopy (LIBS) for the purpose of discriminating between samples originating from different sources. Some of the glass sets were also examined by laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS). Refractive index (RI) measurements were also made on all glass samples and the refractive index data was combined with the LIBS and with the LA-ICP-MS data to enhance discrimination. The glass types examined included float glass taken from front and side automobile windows (examined on the non-float side), automobile headlamp glass, automobile side-mirror glass and brown beverage container glass. The largest overall discrimination was obtained by employing RI data in combination with LA-ICP-MS (98.8% discrimination of 666 pairwise comparisons at 95% confidence), while LIBS in combination with RI provided a somewhat lower discrimination (87.2% discrimination of 1122 pairwise comparisons at 95% confidence). Samples of side-mirror glass were less discriminated by LIBS due to a larger variance in emission intensities, while discrimination of side-mirror glass by LA-ICP-MS remained high

Ion-beam analysis of a medieval glass bottle excavated in Gyoer

International Nuclear Information System (INIS)

Uzonyi, I.; Szoboszlai, Z.; Kertesz, Zs.; Simon, A.; Kiss, A.Z.

2008-01-01

) techniques: the particle induced X-ray emission (PIXE) and the particle induced gamma ray emission (PIGE) were used. Measurements were carried out on a small glass piece from the present archaeological find which was not used for the restoration. PIXE analysis was carried out at the Scanning Nuclear Microprobe facility. The sample was irradiated at five different spots by 2 MeV H + beam focused to 2x2 μm 2 spot size and applying scan size of 2x2 mm 2 . The accumulated charge at the sample was ∼0.2 μC. Characteristic X-rays were detected by an ultra thin windowed and a Be windowed Si(Li) detectors, thus elements could be analyzed for the Z≥6 atomic number region with high sensitivity. Characteristic X-ray spectra were evaluated with the PIXEKLM-TPI software package. Efficiency calibration of detectors was based on the NIST 610 glass standard reference material. In the case of the PIGE analysis the samples were irradiated in an isolated vacuum chamber with a 3.8 MeV proton beam of about 5 nA. The accumulated charge at the sample was ∼3 μC. The gamma-rays were detected with a 40 % HPGe detector situated at 90 deg with respect to the beam direction and 20 cm distance from the sample. To calculate the concentrations of Na, Al and Si the same NIST 610 glass standard was used. The analysis revealed that the bottle was made from soda-lime glass. Comparing Na, Mg and Ca values with available literature data, 'similarity' with Venice glass can be stated. However, considering the high Ti, Fe (and Al) concentrations it can be supposed that a relatively low quality vitrifying agent (siliceous material) was used excluding late medieval (15-16th c.) fine Venetian glass. The greenish tint attributable to the high Fe content indicates incomplete decolourization (by MnO) which is also characteristic for lower quality glass products. Therefore, the analytical results does not falsify the hypotheses that the artefact can be a 13th century (supposedly Venice) glass

Chromium Speciation Analysis by Ion Chromatography Coupled ...

African Journals Online (AJOL)

Two methods coupling ion chromatography with inductively coupled plasma - optical emission spectroscopy (ICP-OES) were developed for the simultaneous separation and determination of Cr(III) and Cr(VI) species. In the first method, anion chromatography with sodium bicarbonate/carbonate solution as the eluent was ...

Micro-Raman and micro-XRF analysis of glass beads from the Chungde site, Taiwan

Science.gov (United States)

Liou, Y. S.; Wang, S. C.; Liu, Y. C.

2014-12-01

A large number of ancient glass beads dating back from Late Neolithic Age to early Historical Period (ca. 2300-400 BP) of Taiwan have been uncovered from archaeological sites. These glass beads with variant colors, shapes, and stylistics have long been considered to possess socio-cultural significance. Due to the color and chemical composition of glass bead might be determined by raw materials, fluxing agents, colorants, opacifiers and stabilizers. In addition, ancient glass beads are rare and precious, non-destructive analysis has been employed to decipher about the provenances, manufacturing techniques, and exchange/trade routes. In this work, micro-Raman spectroscopy and micro X-ray fluorescent spectrometer (μ-XRF) were used to examine ten ancient glass beads excavated from the Chungde site, Hualien, Taiwan, dating back to 1500-800 BP, to unravel the mineralogical and chemical compositions. Micro Raman experimental results show that glass and anorthite glass are the main constituents accompanying with trace level of quartz, albite, siderite, ankerite, and amazonite. The Raman Index of Polymerization (Ip) indicate that the sintering temperature of the glass beads is in the range of 1000~1400°C. Furthermore, the chemical compositions are corresponding to the maximum stretching vibration peak wave number (νmax Si-O Stretching) and the maximum bending vibration peak wave number (δmax Si-O Bending), which are essentially consistent with that of the India-Pacific beads. The μ-XRF results indicate the presence of oxides including SiO2, Al2O3, Fe2O3, Na2O, K2O, CaO, MgO, SnO2, TiO2, CuO, etc., and could be classified to high aluminum of soda-lime glass system. According to ternary phase diagram analysis of CaO-K2O-Na2O and K2O-Al2O3-CaO, the ancient glass beads analyzed could be attributed to the India-Pacific beads, and is in accordance with that of Raman spectra. The combination of these facts leads to the conclusion that glass beads obtained from the Chungde

PIXE and light element analysis (C,N) in glass inclusions trapped in meteorites with the nuclear microprobe

International Nuclear Information System (INIS)

Varela, M.E.; Mosbah, M.; Metrich, N.; Duraud, J.P.; Kurat, G.

1999-01-01

Proton-induced X-ray emission (PIXE) and light element analysis have been performed with the nuclear microprobe at the Laboratoire Pierre Suee (Saclay-France) in glass inclusions of the carbonaceous chondrites: Allende, Kaba and Renazzo, and in the achondrite meteorite: Chassigny. Carbon contents in olivine of chondrules are below the nuclear reactions analysis (NRA) detection limit, however, glasses from glass inclusions hosted by these grains, contain an appreciable and highly variable quantities of carbon (200-1600 ppm). This could indicate variable amounts of C trapped during glass inclusion formation. On the other hand, nitrogen is present in highly variable amounts in glasses of both, chondrites and achondrites minerals. Its abundance, correlated with depth from the section surface which suggests loss of N during analyses and therefore the possible existence of a very mobile (volatile?) species. A chondritic Rb/Sr and K/Rb ratio obtained by PIXE analyses in the glass-bearing inclusions of the Chassigny meteorite points towards a primitive source for the glass precursor of Chassigny inclusions

Archaeometric investigation of medieval Bulgarian glasses and sgraffito ceramics by neutron activation analysis

International Nuclear Information System (INIS)

Dzhingova, R.; Kulev, I.

1985-01-01

Instrumental neutron activation analysis was used to determine the content of Au, Ba, Ca, Ce, Cl, Cr, Co, Cs, Cu, Eu, Fe, Hf, La, Lu, Mn, Na, Rb, Sc, Sm, Sr, Ta, Tb, Th, Ti, U, Sb, V and Yb in glass samples excavated from medieval glassworkshops in Pliska and Preslav and in 20 glass finds from Preslav. Sgraffito ceramic samples excavated in Veliko Tarnovo were also analysed and the elements Al, As, Au, Ba, Br, Ce, Co, Cr, Cs, Dy, Eu, Fe, Hf, K, La, Lu, Mg, Mn, Na, Nd, Rb, Sb, Sc, Si, Sm, Ta, Tb, Th, Ti, U, V and Yb were determined. In order to localize the production site of the archaeological finds, the results from the analysis were subjected to cluster analysis, and stepwise discriminant analysis using the program package BMDP. A variety of the production of the medieval glass workshop in Preslav was identified and evaluated. It was proved that a part of the sgraffito ceramics samples have been produced in one and the same place and that the chemical composition might be successfully used to differentiate between the production of two workshops

Application in pesticide analysis: Liquid chromatography - A review of the state of science for biomarker discovery and identification

Science.gov (United States)

Book Chapter 18, titled Application in pesticide analysis: Liquid chromatography - A review of the state of science for biomarker discovery and identification, will be published in the book titled High Performance Liquid Chromatography in Pesticide Residue Analysis (Part of the C...

Direct uranium isotope ratio analysis of single micrometer-sized glass particles

International Nuclear Information System (INIS)

Kappel, Stefanie; Boulyga, Sergei F.; Prohaska, Thomas

2012-01-01

We present the application of nanosecond laser ablation (LA) coupled to a ‘Nu Plasma HR’ multi collector inductively coupled plasma mass spectrometer (MC-ICP-MS) for the direct analysis of U isotope ratios in single, 10–20 μm-sized, U-doped glass particles. Method development included studies with respect to (1) external correction of the measured U isotope ratios in glass particles, (2) the applied laser ablation carrier gas (i.e. Ar versus He) and (3) the accurate determination of lower abundant 236 U/ 238 U isotope ratios (i.e. 10 −5 ). In addition, a data processing procedure was developed for evaluation of transient signals, which is of potential use for routine application of the developed method. We demonstrate that the developed method is reliable and well suited for determining U isotope ratios of individual particles. Analyses of twenty-eight S1 glass particles, measured under optimized conditions, yielded average biases of less than 0.6% from the certified values for 234 U/ 238 U and 235 U/ 238 U ratios. Experimental results obtained for 236 U/ 238 U isotope ratios deviated by less than −2.5% from the certified values. Expanded relative total combined standard uncertainties U c (k = 2) of 2.6%, 1.4% and 5.8% were calculated for 234 U/ 238 U, 235 U/ 238 U and 236 U/ 238 U, respectively. - Highlights: ► LA-MC-ICP-MS was fully validated for the direct analysis of individual particles. ► Traceability was established by using an IRMM glass particle reference material. ► Measured U isotope ratios were in agreement with the certified range. ► A comprehensive total combined uncertainty evaluation was performed. ► The analysis of 236 U/ 238 U isotope ratios was improved by using a deceleration filter.

ANALYSIS AND IDENTIFICATION SPIKING CHEMICAL COMPOUNDS RELATED TO CHEMICAL WEAPON CONVENTION IN UNKNOWN WATER SAMPLES USING GAS CHROMATOGRAPHY AND GAS CHROMATOGRAPHY ELECTRON IONIZATION MASS SPECTROMETRY

Directory of Open Access Journals (Sweden)

Harry Budiman

2010-06-01

Full Text Available The identification and analysis of chemical warfare agents and their degradation products is one of important component for the implementation of the convention. Nowadays, the analytical method for determination chemical warfare agent and their degradation products has been developing and improving. In order to get the sufficient analytical data as recommended by OPCW especially in Proficiency Testing, the spiking chemical compounds related to Chemical Weapon Convention in unknown water sample were determined using two different techniques such as gas chromatography and gas chromatography electron-impact ionization mass spectrometry. Neutral organic extraction, pH 11 organic extraction, cation exchanged-methylation, triethylamine/methanol-silylation were performed to extract the chemical warfare agents from the sample, before analyzing with gas chromatography. The identification of chemical warfare agents was carried out by comparing the mass spectrum of chemicals with mass spectrum reference from the OPCW Central Analytical Database (OCAD library while the retention indices calculation obtained from gas chromatography analysis was used to get the confirmation and supported data of  the chemical warfare agents. Diisopropyl methylphosphonate, 2,2-diphenyl-2-hydroacetic acid and 3-quinuclidinol were found in unknown water sample. Those chemicals were classified in schedule 2 as precursor or reactant of chemical weapons compound in schedule list of Chemical Weapon Convention.   Keywords: gas chromatography, mass spectrometry, retention indices, OCAD library, chemical warfare agents

Analysis of lignans in Magnoliae Flos by turbulent flow chromatography with online solid-phase extraction and high-performance liquid chromatography with tandem mass spectrometry.

Science.gov (United States)

Zhou, Xuan; Chen, Cen; Ye, Xiaolan; Song, Fenyun; Fan, Guorong; Wu, Fuhai

2016-04-01

In this study, a method coupling turbulent flow chromatography with online solid-phase extraction and high-performance liquid chromatography with tandem mass spectrometry was developed for analyzing the lignans in Magnoliae Flos. By the online pretreatment of turbulent flow chromatography solid-phase extraction, the impurities removal and analytes concentration were automatically processed, and the lignans were separated rapidly and well. Seven lignans of Magnoliae Flos including epieudesmin, magnolin, 1-irioresinol-B-dimethyl ether, epi-magnolin, fargesin aschantin, and demethoxyaschantin were identified by comparing their retention behavior, UV spectra, and mass spectra with those of reference substances or literature data. The developed method was validated, and the good results showed that the method was not only automatic and rapid, but also accurate and reliable. The turbulent flow chromatography with online solid-phase extraction and high-performance liquid chromatography with tandem mass spectrometry method holds a high potential to become an effective method for the quality control of lignans in Magnoliae Flos and a useful tool for the analysis of other complex mixtures. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Stress analysis of glass-ceramic insulator and molybdenum cylinders in vacuum tube subassembly

International Nuclear Information System (INIS)

Spears, R.K.

1980-01-01

This study determined the state of stress between molybdenum cylinders and a glass-ceramic insulator of a vacuum tube during cooling when the glass-ceramic coefficient of expansion differed from molybdenum by +-2 x 10 -7 / 0 C. A thermoelastic stress analysis was performed on the vacuum tube subassembly using the finite element method. Two cases, which examined the effect of cooling over a 700 0 C range, were considered. In Case One, the expansion coefficient of the glass-ceramic was 2 x 10 -7 / 0 C less than that of molybdenum while for Case Two, it was 2 x 10 -7 / 0 C greater. For Case One, it was found that the tangential stresses in the insulator were entirely compressive but the maximum principal stresses in the r-z plane were mainly tensile. For Case Two, the tangential stresses were tensile in the insulator as were most of the maximum principal stresses in the r-z plane except for stress in the upper regions of the insulator. The magnitude of the stress at the maximum principal stress location appears to be substantially lower than what has been observed in practice (i.e., cracking of this design had never been a major problem, but it has been observed that if the coefficient of expansion of the glass-ceramic was 2 x 10 -7 / 0 C lower than molybdenum, cracking usually resulted). This analysis showed that the expansion coefficient of the glass-ceramic could be varied quite liberally from molybdenum before the ultimate strength (13,000 lb/in. 2 ) of the glass-ceramic was exceeded

Analysis of elementary process steps in industrial glass melting tanks: some ideas on innovations in industrial glass melting

NARCIS (Netherlands)

Beerkens, R.G.C.

2008-01-01

Conventional industrial glass furnaces show broad glass melt residence time distributions in the melting tanks and average residence times may be up to more than two days for high quality glass products, such as float glass or TV glass, despite the minimum residence times of 8-10 hours (or even less

Surface analysis of thin film coatings on container glass

Energy Technology Data Exchange (ETDEWEB)

Bhargava, A. [GCC Pty Ltd., Jindalee, QLD (Australia); Wood, B. [The University of Queensland, Brisbane, QLD (Australia). Department of Chemistry

1999-12-01

Full text: Container glass is generally coated with a tin oxide layer followed by a coating of polymer. These coatings are believed to improve the mechanical properties of container glass as well as aid in the application of advertising labels to glass. The tin oxide layer on commercial beer bottles has a total thickness of about 15-20nm which consists of an interfacial layer comprising 70-85% of the total thickness. The polymer coating is about 2-5nm thick and also possesses an interfacial layer with tin oxide. A PHI Model 560 XPS/ SAM/ SIMS multi-technique system Is used to estimate concentration profiles of Sn, O, C, Si, Ca, Na and O. A combination of XPS, AES and SIMS is necessary to describe the coatings. Instrumental conditions and sample preparation methods are developed to optimize the analysis of thin films on glass. The coating comprises of three areas, namely (A) where polymer and tin co-exist (B) a pure tin oxide layer and (C) where tin co-exists with glass. By varying the chemical source of tin, it is possible to systematically vary the thickness of the interface and the concentration profile of Sn. Using XRD, crystalline phase(s) could be detected in tin oxide films as thin as 15nm. While the principle phase is cassiterite, a second phase is also detected which is believed to originate from the interface. Using a UMIS 2000 nanoindentor system, instrumental parameters are optimized for measurement of elastic modulus of films at varying depths, i.e. from surface of coating to the bulk of the glass. A sharp rise is observed at depth corresponding to the interface which is indicative of the significance of the interfacial layer. Samples are prepared by systematic ion-milling which are representative of various regions of the coating, namely (A), (B) and (C). These samples are analyzed by XRD and TEM. Based on these studies, a structural model of tin oxide layer and interface is presented to explain increase in elastic modulus at the interface. Copyright

Surface analysis of thin film coatings on container glass

International Nuclear Information System (INIS)

Bhargava, A.; Wood, B.

1999-01-01

Full text: Container glass is generally coated with a tin oxide layer followed by a coating of polymer. These coatings are believed to improve the mechanical properties of container glass as well as aid in the application of advertising labels to glass. The tin oxide layer on commercial beer bottles has a total thickness of about 15-20nm which consists of an interfacial layer comprising 70-85% of the total thickness. The polymer coating is about 2-5nm thick and also possesses an interfacial layer with tin oxide. A PHI Model 560 XPS/ SAM/ SIMS multi-technique system Is used to estimate concentration profiles of Sn, O, C, Si, Ca, Na and O. A combination of XPS, AES and SIMS is necessary to describe the coatings. Instrumental conditions and sample preparation methods are developed to optimize the analysis of thin films on glass. The coating comprises of three areas, namely (A) where polymer and tin co-exist (B) a pure tin oxide layer and (C) where tin co-exists with glass. By varying the chemical source of tin, it is possible to systematically vary the thickness of the interface and the concentration profile of Sn. Using XRD, crystalline phase(s) could be detected in tin oxide films as thin as 15nm. While the principle phase is cassiterite, a second phase is also detected which is believed to originate from the interface. Using a UMIS 2000 nanoindentor system, instrumental parameters are optimized for measurement of elastic modulus of films at varying depths, i.e. from surface of coating to the bulk of the glass. A sharp rise is observed at depth corresponding to the interface which is indicative of the significance of the interfacial layer. Samples are prepared by systematic ion-milling which are representative of various regions of the coating, namely (A), (B) and (C). These samples are analyzed by XRD and TEM. Based on these studies, a structural model of tin oxide layer and interface is presented to explain increase in elastic modulus at the interface. Copyright

Quantitative analysis of deuterium by gas chromatography

International Nuclear Information System (INIS)

Isomura, Shohei; Kaetsu, Hayato

1981-01-01

An analytical method for the determination of deuterium concentration in water and hydrogen gas by gas chromatography is described. HD and D 2 in a hydrogen gas sample were separated from H 2 by a column packed with Molecular Sieve 13X, using extra pure hydrogen gas as carrier. A thermal conductivity detector was used. Concentrations of deuterium were determined by comparison with standard samples. The error inherent to the present method was less a 1% on the basis of the calibration curves obtained with the standard samples. The average time required for the analysis was about 3 minutes. (author)

Clinical applications of fast liquid chromatography: a review on the analysis of cardiovascular drugs and their metabolites.

Science.gov (United States)

Baranowska, Irena; Magiera, Sylwia; Baranowski, Jacek

2013-05-15

One of the major challenges facing the medicine today is developing new therapies that enhance human health. To help address these challenges the utilization of analytical technologies and high-throughput automated platforms has been employed; in order to perform more experiments in a shorter time frame with increased data quality. In the last decade various analytical strategies have been established to enhance separation speed and efficiency in liquid chromatography applications. Liquid chromatography is an increasingly important tool for monitoring drugs and their metabolites. Furthermore, liquid chromatography has played an important role in pharmacokinetics and metabolism studies at these drug development stages since its introduction. This paper provides an overview of current trends in fast chromatography for the analysis of cardiovascular drugs and their metabolites in clinical applications. Current trends in fast liquid chromatographic separations involve monolith technologies, fused-core columns, high-temperature liquid chromatography (HTLC) and ultra-high performance liquid chromatography (UHPLC). The high specificity in combination with high sensitivity makes it an attractive complementary method to traditional methodology used for routine applications. The practical aspects of, recent developments in and the present status of fast chromatography for the analysis of biological fluids for therapeutic drug and metabolite monitoring, pharmacokinetic studies and bioequivalence studies are presented. Copyright © 2013 Elsevier B.V. All rights reserved.

Immunochromatographic diagnostic test analysis using Google Glass.

Science.gov (United States)

Feng, Steve; Caire, Romain; Cortazar, Bingen; Turan, Mehmet; Wong, Andrew; Ozcan, Aydogan

2014-03-25

We demonstrate a Google Glass-based rapid diagnostic test (RDT) reader platform capable of qualitative and quantitative measurements of various lateral flow immunochromatographic assays and similar biomedical diagnostics tests. Using a custom-written Glass application and without any external hardware attachments, one or more RDTs labeled with Quick Response (QR) code identifiers are simultaneously imaged using the built-in camera of the Google Glass that is based on a hands-free and voice-controlled interface and digitally transmitted to a server for digital processing. The acquired JPEG images are automatically processed to locate all the RDTs and, for each RDT, to produce a quantitative diagnostic result, which is returned to the Google Glass (i.e., the user) and also stored on a central server along with the RDT image, QR code, and other related information (e.g., demographic data). The same server also provides a dynamic spatiotemporal map and real-time statistics for uploaded RDT results accessible through Internet browsers. We tested this Google Glass-based diagnostic platform using qualitative (i.e., yes/no) human immunodeficiency virus (HIV) and quantitative prostate-specific antigen (PSA) tests. For the quantitative RDTs, we measured activated tests at various concentrations ranging from 0 to 200 ng/mL for free and total PSA. This wearable RDT reader platform running on Google Glass combines a hands-free sensing and image capture interface with powerful servers running our custom image processing codes, and it can be quite useful for real-time spatiotemporal tracking of various diseases and personal medical conditions, providing a valuable tool for epidemiology and mobile health.

Density of mixed alkali borate glasses: A structural analysis

International Nuclear Information System (INIS)

Doweidar, H.; El-Damrawi, G.M.; Moustafa, Y.M.; Ramadan, R.M.

2005-01-01

Density of mixed alkali borate glasses has been correlated with the glass structure. It is assumed that in such glasses each alkali oxide associates with a proportional quantity of B 2 O 3 . The number of BO 3 and BO 4 units related to each type of alkali oxide depends on the total concentration of alkali oxide. It is concluded that in mixed alkali borate glasses the volumes of structural units related to an alkali ion are the same as in the corresponding binary alkali borate glass. This reveals that each type of alkali oxide forms its own borate matrix and behaves as if not affected with the presence of the other alkali oxide. Similar conclusions are valid for borate glasses with three types of alkali oxide

The properties of the wood-polystyrene interphase determined by inverse gas chromatography

Science.gov (United States)

John Simonsen; Zhenqiu Hong; Timothy G. Rials

1997-01-01

The properties of the interphase in wood-polymer composites are important determinants of the properties of the final composite. This study used inverse gas chromatography (IGC) to measure interphasal properties of composites of polystyrene and two types of wood fiber fillers and an inoranic substrate (CW) with varying amounts of surface coverage of polystyrene. Glass...

Numerical analysis of historical change of the electric resistance in the TVF glass melter

International Nuclear Information System (INIS)

Kawamura, Takumi; Sakai, Takaaki

2004-09-01

Concerning to the TVF glass melter in the Tokai reprocessing center, it is being planned to detect the deposition of the noble metals in a glass melter and remove them periodically to extend the melter lifetime. Numerical analysis has been performed for the electric resistance evaluation in order to estimate the sedimentation situation and current density distribution from the melter resistance. Electric field analysis was carried out by using MAGNA-FIM code and the influence factors to melter resistance was evaluated concerning to the sedimentation situation and glass temperature. In addition, transitions of the sedimentation and melter resistances were estimated from the operation history of the TVF-1 melter. As a result, the followings were obtained. From the evaluation of the influence factors to melter resistance, it turns out that the volume and the noble metals concentration of a sediment influence notably to melter resistance when the sediment contacts to electrodes. The sediment temperature at the melter bottom has small sensitivity in case of the non-contact situation. The glass temperature in the melter upper part, however, has big sensitivity in melter resistance irrespective of the existence of contact. Based on the above sensitivity evaluation, Numerical analysis was carried out supposing the sedimentation process which suits to a melter resistance fall during the operation history of the TVF-1 melter. As input conditions, the voltage between electrodes and the temperature in the melter were referred from the operation history data. It was assumed that the noble metals concentration in a sediment increased constantly for every operation batch. As a result, the characteristics of melter resistance history was reproduced successfully in general. Thereby, it became prospective to predict the sedimentation situation by using the new resistance analysis model for the glass melter. (author)

Application of Kissinger analysis to glass transition and study of ...

Indian Academy of Sciences (India)

Home; Journals; Bulletin of Materials Science; Volume 35; Issue 4. Application of Kissinger analysis to glass transition and study of thermal degradation kinetics of phenolic–acrylic IPNs ... Author Affiliations. S Goswami1 K Kiran1. Department of Polymer Engineering, Birla Institute of Technology, Ranchi 835 215, India ...

[High-performance liquid-liquid chromatography in beverage analysis].

Science.gov (United States)

Bricout, J; Koziet, Y; de Carpentrie, B

1978-01-01

Liquid liquid chromatography was performed with columns packed with stationary phases chemically bonded to silica microparticules. These columns show a high efficiency and are used very easily. Flavouring compounds like aromatic aldehydes which have a low volatility were analyzed in brandy using a polar phase alkylnitrile. Sapid substances like amarogentin in Gentiana lutea or glyryrrhizin in Glycyrrhiza glabra were determined by reversed phase chromatography. Finally ionizable substances like synthetic dyes can be analyzed by paired ion chromatography witha non polar stationary phase.

Spectrophotometric study of bio-sorption of uranium on glass grade spodumene shell powder

International Nuclear Information System (INIS)

Parakudyil, A.S.; Pillai, A.K.; Reddy, A.V.R.; Singal, R.K.; Sharma, P.K.; Michael, K.M.

2012-01-01

Separation of uranium found in iron ore leachates was done by extraction chromatography using glass grade spodumene shellpowder (GSS) in nitric acid medium and analyzed spectrophotometrically. The influences of metal ion concentration, pH and adsorption capacity of biomass were investigated. Biosorption is a potential method of separation of heavy and trace metals from waste water and effluents from various sources. The adsorption capacities of biomass were investigated by batch experiments and column experiments. In the present study, glass grade spodumene shell powder (GSS) in acidic medium is being used as a biosorbent

Illicit Drug Analysis Using Two-Dimension Liquid Chromatography/Tandem Mass Spectrometry.

Science.gov (United States)

Mallet, Claude; Botch-Jones, Sabra

2016-10-01

For the identification of illicit drugs in forensic toxicological casework, analysis can be delayed and potentially compromised due to lengthy sample preparation techniques. For a complete forensic identification, a robust methodology is required and the current trend in forensic laboratories is the use of liquid chromatography coupled to mass spectrometry (LC/MS or LC/MS-MS). However, to achieve satisfactory results, extensive and time-consuming sample preparation protocols are required to reach sub-ng/mL levels. The concept of sequential 2D extraction was designed to capture the retention behavior of a target analyte in response to various extraction parameters. Therefore, optimized conditions can be selected to excise a region of interest during extraction. The utilization of multi-dimensional chromatography combined with a micro-extraction technique was evaluated to decrease sample preparation time while enhancing the separation integrity observed with current single-dimensional chromatography techniques. A wide range of illicit drugs were spiked in human urine and extracted using three extraction protocols for performance evaluation. The extraction process was performed using a reversed-phase solid phase extraction (SPE) in 1D, 2D-optimized, 2D-sequential and cumulative elution modes. The chosen 2D chromatography conditions that were used in this application were identified using a 6 × 6 automated methods development protocol (144 methods total). The extraction of urine samples containing target analytes was completed in less than 20 min. The analysis was performed using 200 µL of the final organic solvent (MeOH) extracts. The limit of detection for all drugs was measured at 100 pg/mL (ppt) from a 1 mL sample volume. Several analytes showed excellent signal at 10 pg/mL (ppt). © The Author 2016. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

Application of Pyrolysis - Gas Chromatography/Mass Spectrometry in Failure Analysis in the Automotive Industry

OpenAIRE

Kusch, Peter (Dr.)

2015-01-01

This book chapter describes application examples of gas chromatography/mass spectrometry and pyrolysis – gas chromatography/mass spectrometry in failure analysis for the identification of chemical materials like mineral oils and nitrile rubber gaskets. Furthermore, failure cases demanding identification of polymers/copolymers in fouling on the compressor wall of a car air conditioner and identification of fouling on the surface of a bearing race from the automotive industry are demonstr...

Improvement of recovery and repeatability in liquid chromatography-mass spectrometry analysis of peptides

NARCIS (Netherlands)

van Midwoud, Paul M.; Rieux, Laurent; Bischoff, Rainer; Verpoorte, Elisabeth; Niederlander, Harm A. G.

2007-01-01

Poor repeatability of peak areas is a problem frequently encountered in peptide analysis with nanoLiquid Chromatography coupled on-line with Mass Spectrometry (nanoLC-MS). As a result, quantitative analysis will be seriously hampered unless the observed variability can be corrected in some way.

Control of high-level radioactive waste-glass melters

International Nuclear Information System (INIS)

Bickford, D.F.; Coleman, C.J.

1990-01-01

The Defense Waste Processing Facility (DWPF) will immobilize Savannah River Site High Level Waste as a durable borosilicate glass for permanent disposal in a repository. The DWPF will be controlled based on glass composition. The following discussion is a preliminary analysis of the capability of the laboratory methods that can be used to control the glass composition, and the relationships between glass durability and glass properties important to glass melting. The glass durability and processing properties will be controlled by controlling the chemical composition of the glass. The glass composition will be controlled by control of the melter feed transferred from the Slurry Mix Evaporator (SME) to the Melter Feed Tank (MFT). During cold runs, tests will be conducted to demonstrate the chemical equivalence of glass sampled from the pour stream and glass removed from cooled canisters. In similar tests, the compositions of glass produced from slurries sampled from the SME and MFT will be compared to final product glass to determine the statistical relationships between melter feed and glass product. The total error is the combination of those associated with homogeneity in the SME or MFT, sampling, preparation of samples for analysis, instrument calibration, analysis, and the composition/property model. This study investigated the sensitivity of estimation of property data to the combination of variations from sampling through analysis. In this or a similar manner, the need for routine glass product sampling will be minimized, and glass product characteristics will be assured before the melter feed is committed to the melter

[Quantitative determination of glass content in monazite glass-ceramics by IR technique].

Science.gov (United States)

He, Yong; Zhang, Bao-min

2003-04-01

Monazite glass-ceramics consist of both monazite and metaphoshate glass phases. The absorption bands of both phases do not overlap each other, and the absorption intensities of bands 1,275 and 616 cm-1 vary with the glass contents. The correlation coefficient between logarithmic absorbance ratio of the two bands and glass contents was r = 0.9975 and its regression equation was y = 48.356 + 25.93x. The absorbance ratio of bands 952 and 616 cm-1 also varied with different ratios of Ce2O3/La2O3 in synthetic monazites, with r = 0.9917 and a regression equation y = 0.2211 exp (0.0221x). High correlation coefficients show that the IR technique could find new application in the quantitative analysis of glass content in phosphate glass-ceramics.

The effect of aqueous media on the mechanical properties of fluorapatite-mullite glass-ceramics.

Science.gov (United States)

Mollazadeh, S; Ajalli, Siamak; Kashi, Tahereh S Jafarzadeh; Yekta, Bijan Eftekhai; Javadpour, Jafar; Jafari, S; Youssefi, Abbas; Fazel, Akbar

2015-11-01

To verify the effects of alternating thermal changes in aqueous media and chemical composition on mechanical properties of apatite-mullite glass-ceramics and to investigate concentration of ions eluted from glass-ceramics in aqueous media. The glass compositions were from SiO2Al2O3P2O5CaOTiO2BaOZrO2CaF2 system. Glass-ceramics were prepared by heat-treating at 1100°C for 3h samples alternately immersed in water at 5 and 60°C. The 3-point bending strength (n=10) were determined using 3×4×25mm/bar and a universal testing machine, at a cross-head speed of 0.1mm/min. Vickers micro hardness were evaluated by applying a total of 15-20 indentations under a 100g load for 30s. Concentrations of ions eluted from glass-ceramics immersed in 60±5°C double distilled water were determined by ion chromatography. The toxicity of glass-ceramics was assessed by seeding the osteosarcoma cells (MG63) on powder for different days and their cell proliferation assessment was investigated by MTT assay. The data were analyzed using one way analysis of variance and the means were compared by Tukey's test (5% significance level). The highest flexural strength and hardness values after thermal changes belonged to TiO2 and ZrO2 containing glass-ceramics which contained lower amount of released ions. BaO containing glass-ceramic and sample with extra amount of silica showed the highest amount of reduction in their mechanical strength values. These additives enhanced the concentration of eluted ions in aqueous media. MTT results showed that glass-ceramics were almost equivalent concerning their in-vitro biological behavior. Thermal changes and chemical compositions had significant effects on flexural strength and Vickers micro-hardness values. Copyright © 2015 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Forensic analysis of tempered sheet glass by particle induced X-ray emission (PIXE)

Energy Technology Data Exchange (ETDEWEB)

Jisonna, L.J. [Department of Chemistry and Department of Physics, Hope College, Holland, MI 49422-9000 (United States); DeYoung, P.A., E-mail: deyoung@hope.ed [Department of Chemistry and Department of Physics, Hope College, Holland, MI 49422-9000 (United States); Ferens, J.; Hall, C.; Lunderberg, J.M.; Mears, P. [Department of Chemistry and Department of Physics, Hope College, Holland, MI 49422-9000 (United States); Padilla, D. [Department of Physics, San Diego State University, San Diego, CA 92182-1233 (United States); Peaslee, G.F. [Department of Chemistry and Department of Physics, Hope College, Holland, MI 49422-9000 (United States); Sampson, R. [Department of Physics, Columbia University, New York, NY 10027 (United States)

2011-05-15

Highlights: {yields} PIXE was found to give the same results for trace elements in glass as ICP. {yields} PIXE can non-destructively determine trace element concentrations in auto glass. {yields} Measured Ca, Fe, Ti, Mn, and Sr in auto glass with PIXE. -- Abstract: The elemental concentrations of five trace elements in tempered sheet glass fragments were determined using particle-induced X-ray emission (PIXE) spectrometry. The trace element concentrations for calcium, iron, manganese, strontium, and titanium are compared to those obtained by inductively-coupled plasma-atomic emission spectrometry (ICP-AES) following complete digestion by hydrofluoric acid. For these five elements, the absolute concentrations obtained by both methods are shown to agree well over a wide range of concentrations. The limits of detection for trace elements are typically lower for the ICP-AES method. However, we show that the concentrations of these five elements can be accurately measured by the PIXE method. Since PIXE is an entirely non-destructive method, there exists a niche for this technique to be used as a complement to the more sensitive ICP-AES technique in the forensic analysis of sheet glass.

High-performance liquid ion-pair chromatography in inorganic analysis

International Nuclear Information System (INIS)

Alimarin, I.P.; Basova, E.M.; Bol'shova, T.A.; Ivanov, V.M.

1990-01-01

In literature review for the recent 15 years theoretical foundations, regularities and mechanisms of ionized compound retention in reverse-phase ion-pair chromatography are considered, possibilities and prospects of its application in inorganic analysis being demonstrated. Analytic characteristics of the methods for the determination of inorganic anions (I - , IO 3 - , MoO 4 2- , etc.), as well as metals (Zr, Hf, V, Nb, Mo, W, Ru, lanthanides, etc.) in the form of chelates, are given

Quantitative analysis of target components by comprehensive two-dimensional gas chromatography

NARCIS (Netherlands)

Mispelaar, V.G. van; Tas, A.C.; Smilde, A.K.; Schoenmakers, P.J.; Asten, A.C. van

2003-01-01

Quantitative analysis using comprehensive two-dimensional (2D) gas chromatography (GC) is still rarely reported. This is largely due to a lack of suitable software. The objective of the present study is to generate quantitative results from a large GC x GC data set, consisting of 32 chromatograms.

The analysis of carbohydrates in milk powder by a new "heart-cutting" two-dimensional liquid chromatography method.

Science.gov (United States)

Ma, Jing; Hou, Xiaofang; Zhang, Bing; Wang, Yunan; He, Langchong

2014-03-01

In this study, a new"heart-cutting" two-dimensional liquid chromatography method for the simultaneous determination of carbohydrate contents in milk powder was presented. In this two dimensional liquid chromatography system, a Venusil XBP-C4 analysis column was used in the first dimension ((1)D) as a pre-separation column, a ZORBAX carbohydrates analysis column was used in the second dimension ((2)D) as a final-analysis column. The whole process was completed in less than 35min without a particular sample preparation procedure. The capability of the new two dimensional HPLC method was demonstrated in the determination of carbohydrates in various brands of milk powder samples. A conventional one dimensional chromatography method was also proposed. The two proposed methods were both validated in terms of linearity, limits of detection, accuracy and precision. The comparison between the results obtained with the two methods showed that the new and completely automated two dimensional liquid chromatography method is more suitable for milk powder sample because of its online cleanup effect involved. Crown Copyright © 2013. Published by Elsevier B.V. All rights reserved.

Determination of residual boron in thermally treated controlled-porosity glasses, by colorimetry, spectrography and isotachophoresis

International Nuclear Information System (INIS)

Dawidowicz, A.L.; Matusewicz, J.; Wysocka-Lisek, J.

1989-01-01

Controlled-porosity glasses (CPGs) are often applied as sorbents in chromatography. Besides having high thermal, chemical and mechanical resistance they are characterized by a very narrow pore-size distribution and the choice of mean pore diameter and porosity covers a wide range. In spite of these advantages, their range of use in chromatography is restricted because of their strong adsorption properties, which are connected with the presence of residual boron atoms in the porous CPG skeleton. The boron concentration on the CPG surface can be increased by proper thermal treatment. When CPGs are heated in the range 400-800 0 the residual boron atoms in the network diffuse from the bulk to the surface. The paper discusses the boron content in porous glasses of different mean pore diameters and the determination of the enrichment of boron on the GPG surface, by three independent methods: colorimetry, spectrography and isotachophoresis. (author)

Wavelength dependence on the forensic analysis of glass by nanosecond 266 nm and 1064 nm laser induced breakdown spectroscopy

Energy Technology Data Exchange (ETDEWEB)

Cahoon, Erica M.; Almirall, Jose R.

2010-05-01

Laser induced breakdown spectroscopy can be used for the chemical characterization of glass to provide evidence of an association between a fragment found at a crime scene to a source of glass of known origin. Two different laser irradiances, 266 nm and 1064 nm, were used to conduct qualitative and quantitative analysis of glass standards. Single-pulse and double-pulse configurations and lens-to-sample-distance settings were optimized to yield the best laser-glass coupling. Laser energy and acquisition timing delays were also optimized to result in the highest signal-to-noise ratio corresponding to the highest precision and accuracy. The crater morphology was examined and the mass removed was calculated for both the 266 nm and 1064 nm irradiations. The analytical figures of merit suggest that the 266 nm and 1064 nm wavelengths are capable of good performance for the forensic chemical characterization of glass. The results presented here suggest that the 266 nm laser produces a better laser-glass matrix coupling, resulting in a better stoichiometric representation of the glass sample. The 266 nm irradiance is therefore recommended for the forensic analysis and comparison of glass samples.

Wavelength dependence on the forensic analysis of glass by nanosecond 266 nm and 1064 nm laser induced breakdown spectroscopy

International Nuclear Information System (INIS)

Cahoon, Erica M.; Almirall, Jose R.

2010-01-01

Laser induced breakdown spectroscopy can be used for the chemical characterization of glass to provide evidence of an association between a fragment found at a crime scene to a source of glass of known origin. Two different laser irradiances, 266 nm and 1064 nm, were used to conduct qualitative and quantitative analysis of glass standards. Single-pulse and double-pulse configurations and lens-to-sample-distance settings were optimized to yield the best laser-glass coupling. Laser energy and acquisition timing delays were also optimized to result in the highest signal-to-noise ratio corresponding to the highest precision and accuracy. The crater morphology was examined and the mass removed was calculated for both the 266 nm and 1064 nm irradiations. The analytical figures of merit suggest that the 266 nm and 1064 nm wavelengths are capable of good performance for the forensic chemical characterization of glass. The results presented here suggest that the 266 nm laser produces a better laser-glass matrix coupling, resulting in a better stoichiometric representation of the glass sample. The 266 nm irradiance is therefore recommended for the forensic analysis and comparison of glass samples.

Analysis of viscoelastic flow in tin phosphate glass

International Nuclear Information System (INIS)

Cha, Jaemin; Asida, Yuto; Takebe, Hiromichi

2011-01-01

The change of the viscoelastic flow near the imprinting temperature was analyzed by a penetration method with a commercial TMA and the result was compared with thermally-imprinted SnO-P 2 O 5 (SP) and SnO-B 2 O 3 -P 2 O 5 (SBP) glass samples by an imprint apparatus. The viscosity of SP glass increases monotonically with increasing SnO content and the specific movement is shown in viscoelastic flow under the optimized thermal imprinting temperature for SP glasses.

Comprehensive two-dimensional gas chromatography applied to illicit drug analysis.

Science.gov (United States)

Mitrevski, Blagoj; Wynne, Paul; Marriott, Philip J

2011-11-01

Multidimensional gas chromatography (MDGC), and especially its latest incarnation--comprehensive two-dimensional gas chromatography (GC × GC)--have proved advantageous over and above classic one-dimensional gas chromatography (1D GC) in many areas of analysis by offering improved peak capacity, often enhanced sensitivity and, especially in the case of GC × GC, the unique feature of 'structured' chromatograms. This article reviews recent advances in MDGC and GC × GC in drug analysis with special focus on ecstasy, heroin and cocaine profiling. Although 1D GC is still the method of choice for drug profiling in most laboratories because of its simplicity and instrument availability, GC × GC is a tempting proposition for this purpose because of its ability to generate a higher net information content. Effluent refocusing due to the modulation (compression) process, combined with the separation on two 'orthogonal' columns, results in more components being well resolved and therefore being analytically and statistically useful to the profile. The spread of the components in the two-dimensional plots is strongly dependent on the extent of retention 'orthogonality' (i.e. the extent to which the two phases possess different or independent retention mechanisms towards sample constituents) between the two columns. The benefits of 'information-driven' drug profiling, where more points of reference are usually required for sample differentiation, are discussed. In addition, several limitations in application of MDGC in drug profiling, including data acquisition rate, column temperature limit, column phase orthogonality and chiral separation, are considered and discussed. Although the review focuses on the articles published in the last decade, a brief chronological preview of the profiling methods used throughout the last three decades is given.

Parametric analysis of a solar still with inverted V-shaped glass condenser

Directory of Open Access Journals (Sweden)

Rubio Eduardo

2015-01-01

Full Text Available A parametric analysis of a solar still with an inverted V-shaped glass condenser is presented. Results are based on a new mathematical model obtained from a lumped-parameter analysis of the still, with an approach that makes each glass plate of the condensing system sensitive to orientation and depicts its thermal differences. Numerical computations are made to evaluate productivity and temperature differences between the condensing plates as a function of condenser orientation, extinction coefficient and thickness. From this study it was found a significant influence of incident solar radiation on the thermal performance of each condensing plate. Large extinction coefficients and thick glass plates increase absorption losses that result in an appreciable temperature difference. An extinction coefficient of 40 m-1 produces a temperature difference of 2.5°C between both condensers. A glass thickness of 10 mm may increase this temperature difference up to 3.5°C. With respect to the production, due to the still orientation, a difference of 8.7% was found for the condensing plates facing an east-west direction. The proposed model is able to reproduce the temperature and distillate production differences that arise between both condensers in good agreement with experimental data. The overall performance of the still, studied with this new approach, was also in accordance with the widely used traditional models for solar distillation. In addition, the condensing plates parameters of the still can be used to force a differential heating such that for the whole day the temperature of one condensing plate is always higher.

Polymer brushes: a controllable system with adjustable glass transition temperature of fragile glass formers.

Science.gov (United States)

Xie, Shi-Jie; Qian, Hu-Jun; Lu, Zhong-Yuan

2014-01-28

We present results of molecular dynamics simulations for coarse-grained polymer brushes in a wide temperature range to investigate the factors that affect the glass transition in these systems. We focus on the influences of free surface, polymer-substrate interaction strength, grafting density, and chain length not only on the change of glass transition temperature Tg, but also the fragility D of the glass former. It is found that the confinement can enhance the dependence of the Tg on the cooling rate as compared to the bulk melt. Our layer-resolved analysis demonstrates that it is possible to control the glass transition temperature Tg of polymer brushes by tuning the polymer-substrate interaction strength, the grafting density, and the chain length. Moreover, we find quantitative differences in the influence range of the substrate and the free surface on the density and dynamics. This stresses the importance of long range cooperative motion in glass formers near the glass transition temperature. Furthermore, the string-like cooperative motion analysis demonstrates that there exists a close relation among glass transition temperature Tg, fragility D, and string length ⟨S⟩. The polymer brushes that possess larger string length ⟨S⟩ tend to have relatively higher Tg and smaller D. Our results suggest that confining a fragile glass former through forming polymer brushes changes not only the glass transition temperature Tg, but also the very nature of relaxation process.

Immunoaffinity chromatography for the sample pretreatment of Taxus plant and cell extracts prior to analysis of taxanes by high-performance liquid chromatography

NARCIS (Netherlands)

Theodoridis, G; Haasnoot, W; Schilt, R; Jaziri, M; Diallo, B; Papadoyannis, IN; de Jong, GJ; Cazemier, G.

2002-01-01

The application of immunoaffinity chromatography for the purification of Taxus plant and cell extracts prior to the HPLC analysis is described. Polyclonal antibodies raised against 10-deacetylbaccatin III (10-DAB III), paclitaxel's main precursor in plant, were characterised by enzymed-linked

Frequency and deflection analysis of cenosphere/glass fiber interply hybrid composite cantilever beam

Science.gov (United States)

Bharath, J.; Joladarashi, Sharnappa; Biradar, Srikumar; Kumar, P. Naveen

2018-04-01

Interply hybrid laminates contain plies made of two or more different composite systems. Hybrid composites have unique features that can be used to meet specified design requirements in a more cost-effective way than nonhybrid composites. They offer many advantages over conventional composites including balanced strength and stiffness, enhanced bending and membrane mechanical properties, balanced thermal distortion stability, improved fatigue/impact resistance, improved fracture toughness and crack arresting properties, reduced weight and cost. In this paper an interply hybrid laminate composite containing Cenosphere reinforced polymer composite core and glass fiber reinforced polymer composite skin is analysied and effect of volume fraction of filler on frequency and load v/s deflection of hybrid composite are studied. Cenosphere reinforced polymer composite has increased specific strength, specific stiffness, specific density, savings in cost and weight. Glass fiber reinforced polymer composite has higher torsional rigidity when compared to metals. These laminate composites are fabricated to meet several structural applications and hence there is a need to study their vibration and deflection properties. Experimental investigation starts with fabrication of interply hybrid composite with cores of cenosphere reinforced epoxy composite volume fractions of CE 15, CE 25, CE15_UC as per ASTM E756-05C, and glasss fiber reinforced epoxy skin, cast product of required dimension by selecting glass fibre of proper thickness which is currently 0.25mm E-glass bidirectional woven glass fabric having density 2500kg/m3, in standard from cast parts of size 230mmX230mmX5mm in an Aluminum mould. Modal analysis of cantilever beam is performed to study the variation of natural frequency with strain gauge and the commercially available Lab-VIEW software and deflection in each of the cases by optical Laser Displacement Measurement Sensor to perform Load versus Deflection Analysis

[Column chromatography purification and analysis of biodiesel by transesterification].

Science.gov (United States)

Liu, Yang; Yi, Huai-feng; Chen, Yu; Wu, Yu-long; Yang, Ming-de; Chen, Zeng; Tong, Jun-mao

2012-02-01

In the present paper, crude biodiesel prepared with sorbifolia oil as raw material by transesterification was purified by column chromatography, then the composition of biodiesel was analyzed by gas chromatography, FTIR, GC-MS and 1H NMR. Column chromatography can separate the crude biodiesel into two fractions: petroleum ether eluted fraction (A1) and methanol eluted fraction (A2). Petroleum ether eluted fraction was mainly biodiesel fraction, which was produced from sorbifolia oil by transesterification, including methyl linoleate, methyl cis-9-octadecenoate and so on; methanol eluted fraction was mainly glycerol fraction, which came from the side reaction of transesterification. The results show that the purity of refined biodiesel increased from 77.51% to 93.872, and the product recovery rate reached up to 91.04% after the purification by column chromatography. The results obtained by FTIR and 1H NMR further showed that the column chromatography can effectively improve the purity of biodiesel. This paper provides a basis for industrialization of purification of biodiesel.

Analysis of bioactive glasses obtained by sol-gel processing for radioactive implants

Directory of Open Access Journals (Sweden)

Roberto Wanderley dos Santos

2003-01-01

Full Text Available This paper presents the chemical and physical characterizations of SiO2 and SiO2-CaO bioactive glasses incorporated with samarium atoms, produced by sol-gel synthesis. The objective is to provide biocompatible and biodegradable radioactive seeds as an alternative to be used in Brachytherapy for the treatment of prostate cancer. The glasses were produced and analyzed by X-ray fluorescence spectroscopy (XRF, energy dispersive X-ray spectroscopy (EDS, scanning electron microscopy (SEM, He picnometry and nitrogen adsorption analysis. A theoretical evaluation of the specific activity of the samples upon neutron activation is proposed. The XRF and EDS results demonstrate the incorporation of samarium atoms in the glass matrix. The experimental data coupled with the theoretical studies in neutron activation suggest that it is possible to obtain radioactive seeds with activities equivalent to 125I seeds used in brachytherapy prostatic.

Field burial results and SIMS analysis of the Chalk River glass blocks

International Nuclear Information System (INIS)

Tait, J.C.; Hocking, W.H.; Betteridge, J.S.; Bart, G.

1986-01-01

In 1959, 25 2-kg hemispherical blocks of aluminosilicate glass, each containing ∼90 MBq/g of mixed fission products, were buried in a sandy soil aquifer in the waste management area at the Chalk River Nuclear Laboratories. A second set of blocks, containing ∼260 MBq/g mixed fission products, was buried in 1960. One block from each test was retrieved in 1978 to undergo chemical and surface analysis. This report reviews the migration of the 90 Sr and 137 Cs plume in the soil and presents the results of SIMS depth profiling of the surface of a glass block. (author)

Mathematical analysis of frontal affinity chromatography in particle and membrane configurations.

Science.gov (United States)

Tejeda-Mansir, A; Montesinos, R M; Guzmán, R

2001-10-30

The scaleup and optimization of large-scale affinity-chromatographic operations in the recovery, separation and purification of biochemical components is of major industrial importance. The development of mathematical models to describe affinity-chromatographic processes, and the use of these models in computer programs to predict column performance is an engineering approach that can help to attain these bioprocess engineering tasks successfully. Most affinity-chromatographic separations are operated in the frontal mode, using fixed-bed columns. Purely diffusive and perfusion particles and membrane-based affinity chromatography are among the main commercially available technologies for these separations. For a particular application, a basic understanding of the main similarities and differences between particle and membrane frontal affinity chromatography and how these characteristics are reflected in the transport models is of fundamental relevance. This review presents the basic theoretical considerations used in the development of particle and membrane affinity chromatography models that can be applied in the design and operation of large-scale affinity separations in fixed-bed columns. A transport model for column affinity chromatography that considers column dispersion, particle internal convection, external film resistance, finite kinetic rate, plus macropore and micropore resistances is analyzed as a framework for exploring further the mathematical analysis. Such models provide a general realistic description of almost all practical systems. Specific mathematical models that take into account geometric considerations and transport effects have been developed for both particle and membrane affinity chromatography systems. Some of the most common simplified models, based on linear driving-force (LDF) and equilibrium assumptions, are emphasized. Analytical solutions of the corresponding simplified dimensionless affinity models are presented. Particular

CRYSTALLIZATION KINETICS OF GLASS-CERAMICS BY DIFFERENTIAL THERMAL ANALYSIS

Directory of Open Access Journals (Sweden)

A. NOZAD

2011-06-01

Full Text Available The crystallization behavior of fluorphlogopite, a glass-ceramic in the MgO–SiO2–Al2O3–K2O–B2O3–F system, was studied by substitution of Li2O for K2O in the glass composition. DTA, XRD and SEM were used for the study of crystallization behavior, formed phases and microstructure of the resulting glass-ceramics. Crystallization kinetics of the glass was investigated under non-isothermal conditions, using the formal theory of transformations for heterogeneous nucleation. The crystallization results were analyzed, and both the activation energy of crystallization process as well as the crystallization mechanism were characterized. Calculated kinetic parameters indicated that the appropriate crystallization mechanism was bulk crystallization for base glass and the sample with addition of Li2O. Non-isothermal DTA experiments showed that the crystallization activation energies of base glasses was in the range of 234-246 KJ/mol and in the samples with addition of Li2O was changed to the range of 317-322 KJ/mol.

Doping control analysis of anabolic steroids in equine urine by gas chromatography-tandem mass spectrometry.

Science.gov (United States)

Wong, April S Y; Leung, Gary N W; Leung, David K K; Wan, Terence S M

2017-09-01

Anabolic steroids are banned substances in equine sports. Gas chromatography-mass spectrometry (GC-MS) has been the traditional technique for doping control analysis of anabolic steroids in biological samples. Although liquid chromatography-mass spectrometry (LC/MS) has become an important technique in doping control, the detection of saturated hydroxysteroids by LC-MS remains a problem due to their low ionization efficiency under electrospray. The recent development in fast-scanning gas-chromatography-triple-quadrupole mass spectrometry (GC-MS/MS) has provided a better alternative with a significant reduction in chemical noise by means of selective reaction monitoring. Herein, we present a sensitive and selective method for the screening of over 50 anabolic steroids in equine urine using gas chromatography-tandem mass spectrometry (GC-MS/MS). Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

Sampling and Analysis Instruction for the 120-F-1 Glass Dump Site

International Nuclear Information System (INIS)

Brown, T.M.

1998-01-01

This sampling and analysis instruction has been prepared to clearly define the sampling and analysis activities to be performed to develop the basis for surveillance and maintenance of the 120-F-1 Glass Dumpsite. The purpose of this investigation is to augment historical information and obtain data to establish a technical basis for surveillance and maintenance at the site

Comparison of ultra high performance supercritical fluid chromatography, ultra high performance liquid chromatography, and gas chromatography for the separation of synthetic cathinones.

Science.gov (United States)

Carnes, Stephanie; O'Brien, Stacey; Szewczak, Angelica; Tremeau-Cayel, Lauriane; Rowe, Walter F; McCord, Bruce; Lurie, Ira S

2017-09-01

A comparison of ultra high performance supercritical fluid chromatography, ultra high performance liquid chromatography, and gas chromatography for the separation of synthetic cathinones has been conducted. Nine different mixtures of bath salts were analyzed in this study. The three different chromatographic techniques were examined using a general set of controlled synthetic cathinones as well as a variety of other synthetic cathinones that exist as positional isomers. Overall 35 different synthetic cathinones were analyzed. A variety of column types and chromatographic modes were examined for developing each separation. For the ultra high performance supercritical fluid chromatography separations, analyses were performed using a series of Torus and Trefoil columns with either ammonium formate or ammonium hydroxide as additives, and methanol, ethanol or isopropanol organic solvents as modifiers. Ultra high performance liquid chromatographic separations were performed in both reversed phase and hydrophilic interaction chromatographic modes using SPP C18 and SPP HILIC columns. Gas chromatography separations were performed using an Elite-5MS capillary column. The orthogonality of ultra high performance supercritical fluid chromatography, ultra high performance liquid chromatography, and gas chromatography was examined using principal component analysis. For the best overall separation of synthetic cathinones, the use of ultra high performance supercritical fluid chromatography in combination with gas chromatography is recommended. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Stability of levothyroxine injection in glass, polyvinyl chloride, and polyolefin containers.

Science.gov (United States)

Frenette, Anne Julie; MacLean, Robert D; Williamson, David; Marsolais, Pierre; Donnelly, Ronald F

2011-09-15

The 24-hour stability of a levothyroxine solution admixed and stored in three common infusion containers and infused through polyvinyl chloride (PVC) tubing was evaluated. Levothyroxine sodium 1-μg/mL injection prepared in glass bottles and PVC and polyolefin bags were assayed using high-performance liquid chromatography at 0, 1, 3, 6, 12, and 24 hours; samples drawn directly from the containers, as well as from the distal end of attached PVC tubing, were assayed. The area under the time-versus-concentration curve (AUC) for predicted and delivered doses was calculated; analysis of variance was used for comparison of the percentages of predicted and actual AUC values. The levothyroxine concentration was stable in glass bottles and polyolefin bags through 24 hours (mean ± S.D. percentage of initial concentration remaining, 103.5% ± 2.5% and 100.0% ± 2.9%, respectively). In the PVC infusion bags, the amount of drug decreased to 90% of the initial concentration within 1 hour and then rose and remained within acceptability limits. The levothyroxine concentration of the samples infused through PVC line from glass and polyolefin containers decreased after 1 hour by about 13%; the loss of the drug from the samples infused from PVC bags was higher (18%), presumably due to additive adsorptive effects. In all samples tested, the drug concentration rebounded and remained above 90% to the end of the study. Levothyroxine sodium 1-μg/mL solution was stable for 24 hours in glass bottles and polyolefin bags but when stored in PVC bags, the concentration decreased by 10% after 1 hour.

On-line liquid chromatography-gas chromatography: A novel approach for the analysis of phytosterol oxidation products in enriched foods.

Science.gov (United States)

Scholz, Birgit; Wocheslander, Stefan; Lander, Vera; Engel, Karl-Heinz

2015-05-29

A novel methodology for the automated qualitative and quantitative determination of phytosterol oxidation products in enriched foods via on-line liquid chromatography-gas chromatography (LC-GC) was established. The approach is based on the LC pre-separation of acetylated phytosterols and their corresponding oxides using silica as stationary phase and a mixture of n-hexane/methyl tert-butyl ether/isopropanol as eluent. Two LC-fractions containing (i) 5,6-epoxy- and 7-hydroxyphytosterols, and (ii) 7-ketophytosterols are transferred on-line to the GC for the analysis of their individual compositions on a medium polar trifluoropropylmethyl polysiloxane capillary column. Thus, conventionally employed laborious off-line purification and enrichment steps can be avoided. Validation data, including recovery, repeatability, and reproducibility of the method, were elaborated using an enriched margarine as example. The margarine was subjected to a heating procedure in order to exemplarily monitor the formation of phytosterol oxidation products. Quantification was performed using on-line LC-GC-FID, identification of the analytes was based on on-line LC-GC-MS. The developed approach offers a new possibility for the reliable and fast analysis of phytosterol oxidation products in enriched foods. Copyright © 2015 Elsevier B.V. All rights reserved.

Comprehensive two-dimensional gas chromatography for the analysis of organohalogenated micro-contaminants

NARCIS (Netherlands)

Korytar, P.; Haglund, P.; Boer, de J.; Brinkman, U.A.Th.

2006-01-01

We explain the principles of comprehensive two-dimensional gas chromatography (GC × GC), and discuss key instrumental aspects - with emphasis on column combinations and mass spectrometric detection. As the main item of interest, we review the potential of GC × GC for the analysis of

Iron phosphate glass containing simulated fast reactor waste: Characterization and comparison with pristine iron phosphate glass

International Nuclear Information System (INIS)

Joseph, Kitheri; Asuvathraman, R.; Venkata Krishnan, R.; Ravindran, T.R.; Govindaraj, R.; Govindan Kutty, K.V.; Vasudeva Rao, P.R.

2014-01-01

Detailed characterization was carried out on an iron phosphate glass waste form containing 20 wt.% of a simulated nuclear waste. High temperature viscosity measurement was carried out by the rotating spindle method. The Fe 3+ /Fe ratio and structure of this waste loaded iron phosphate glass was investigated using Mössbauer and Raman spectroscopy respectively. Specific heat measurement was carried out in the temperature range of 300–700 K using differential scanning calorimeter. Isoconversional kinetic analysis was employed to understand the crystallization behavior of the waste loaded iron phosphate glass. The glass forming ability and glass stability of the waste loaded glass were also evaluated. All the measured properties of the waste loaded glass were compared with the characteristics of pristine iron phosphate glass

Recycle Glass in Foam Glass Production

DEFF Research Database (Denmark)

Petersen, Rasmus Rosenlund; König, Jakob; Yue, Yuanzheng

The foam glass industry turn recycle glass into heat insulating building materials. The foaming process is relative insensitive to impurities in the recycle glass. It is therefore considered to play an important role in future glass recycling. We show and discuss trends of use of recycled glasses...... in foam glass industry and the supply sources and capacity of recycle glass....

Isotope effect in glass-transition temperature and ionic conductivity of lithium-borate glasses

International Nuclear Information System (INIS)

Nagasaki, Takanori; Morishima, Ryuta; Matsui, Tsuneo

2002-01-01

The glass-transition temperature and the electrical conductivity of lithium borate (0.33Li 2 O-0.67B 2 O 3 ) glasses with various isotopic compositions were determined by differential thermal analysis and by impedance spectroscopy, respectively. The obtained glass-transition temperature as well as the vibrational frequency of B-O network structure was independent of lithium isotopic composition. This result indicates that lithium ions, which exist as network modifier, only weakly interact with B-O network structure. In addition, the glass-transition temperature increased with 10 B content although the reason has not been understood. The electrical conductivity, on the other hand, increased with 6 Li content. The ratio of the conductivity of 6 Li glass to that of 7 Li glass was found to be 2, being larger than the value (7/6) 1/2 calculated with the simple classical diffusion theory. This strong mass dependence could be explained by the dynamic structure model, which assumes local structural relaxation even far below the glass-transition temperature. Besides, the conductivity appeared to increase with the glass-transition temperature. Possible correlations between the glass-transition temperature and the electrical conductivity were discussed. (author)

High Performance Liquid Chromatography of Some Analgesic Compounds: An Instrumental Analysis Experiment.

Science.gov (United States)

Haddad, Paul; And Others

1983-01-01

Background information, procedures, and results are provided for an experiment demonstrating techniques of solvent selection, gradient elution, pH control, and ion-pairing in the analysis of an analgesic mixture using reversed-phase liquid chromatography on an octadecylsilane column. Although developed using sophisticated/expensive equipment, less…

Thermal analysis of a glass bending process

International Nuclear Information System (INIS)

Buonanno, G.; Dell'Isola, M.; Frattolillo, A.; Giovinco, G.

2005-01-01

The paper presents the thermal simulation of naturally ventilated ovens used in glass sheets hot forming for windscreen production. The determination of thermal and flow conditions in the oven and, consequently, the windshield temperature distribution is necessary both for the productive process optimisation and to assure beforehand, without any iterative tuning process, the required characteristics of the product considered. To this purpose, the authors carried out a 3D numerical simulation of the thermal interaction between the glass and the oven internal surfaces during the whole heating process inside the oven. In particular, a finite volumes method was used to take into account both the convective, conductive and radiative heat transfer in the oven. The numerical temperature distribution in the glass was validated through the comparison with the data obtained from an experimental apparatus designed and built for the purpose

Analysis of new psychoactive substances in human urine by ultra-high performance supercritical fluid and liquid chromatography: Validation and comparison.

Science.gov (United States)

Borovcová, Lucie; Pauk, Volodymyr; Lemr, Karel

2018-05-01

New psychoactive substances represent serious social and health problem as tens of new compounds are detected in Europe annually. They often show structural proximity or even isomerism, which complicates their analysis. Two methods based on ultra high performance supercritical fluid chromatography and ultra high performance liquid chromatography with mass spectrometric detection were validated and compared. A simple dilute-filter-and-shoot protocol utilizing propan-2-ol or methanol for supercritical fluid or liquid chromatography, respectively, was proposed to detect and quantify 15 cathinones and phenethylamines in human urine. Both methods offered fast separation (chromatography. Limits of detection in urine ranged from 0.01 to 2.3 ng/mL, except for cathinone (5 ng/mL) in supercritical fluid chromatography. Nevertheless, this technique distinguished all analytes including four pairs of isomers, while liquid chromatography was unable to resolve fluoromethcathinone regioisomers. Concerning matrix effects and recoveries, supercritical fluid chromatography produced more uniform results for different compounds and at different concentration levels. This work demonstrates the performance and reliability of supercritical fluid chromatography and corroborates its applicability as an alternative tool for analysis of new psychoactive substances in biological matrixes. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

An all-glass solid sampling device for open tubular columns in gas chromatography

NARCIS (Netherlands)

Cox, T.P.H.; vd Berg, P.M.J.

1972-01-01

An all-glass system for direct sample-introduction of high-boiling compounds onto open tubular columns is described. The standard deviation for quantitative measurements is less than 2.7%. The loss in resolving power of capillary columns, due to this injection system is negligible. The system is

Neural network analysis of nuclear waste glass composition vs durability

International Nuclear Information System (INIS)

Seibel, C.K.

1994-01-01

The relationship between the chemical composition of oxide glasses and their physical properties is poorly understood, but it is becoming more important as vitrification (transformation into glass) of high-level nuclear waste becomes the favored method for long-term storage. The vitrified waste will be stored deep in geologic repositories where it must remain intact for at least 10,000 years. A strong resistance to groundwater exposure; i.c. a slow rate of glass dissolution, is of great importance. This project deals specifically with glass samples developed and tested for the nuclear fuel reprocessing facility near West Valley, New York. This facility needs to dispose of approximately 2.2 million liters of high-level radioactive liquid waste currently stored in stainless steel tanks. A self-organizing, artificial neural network was used to analyze the trends in the glass dissolution data for the effects of composition and the resulting durability of borosilicate glasses in an aqueous environment. This durability data can be used to systematically optimize the properties of the complex nuclear glasses and slow the dissolution rate of radionuclides into the environment

Identifying glass compositions in fly ash

Directory of Open Access Journals (Sweden)

Katherine eAughenbaugh

2016-01-01

Full Text Available In this study, four Class F fly ashes were studied with a scanning electron microscope; the glassy phases were identified and their compositions quantified using point compositional analysis with k-means clustering and multispectral image analysis. The results showed that while the bulk oxide contents of the fly ashes were different, the four fly ashes had somewhat similar glassy phase compositions. Aluminosilicate glasses (AS, calcium aluminosilicate glasses (CAS, a mixed glass, and, in one case, a high iron glass were identified in the fly ashes. Quartz and iron crystalline phases were identified in each fly ash as well. The compositions of the three main glasses identified, AS, CAS, and mixed glass, were relatively similar in each ash. The amounts of each glass were varied by fly ash, with the highest calcium fly ash containing the most of calcium-containing glass. Some of the glasses were identified as intermixed in individual particles, particularly the calcium-containing glasses. Finally, the smallest particles in the fly ashes, with the most surface area available to react in alkaline solution, such as when mixed with portland cement or in alkali-activated fly ash, were not different in composition than the large particles, with each of the glasses represented. The method used in the study may be applied to a fly ash of interest for use as a cementing material in order to understand its potential for reactivity.

[Analysis of microalbuminuria with immunonephelometry and high performance liquid chromatography. Evaluation of new criteria].

Science.gov (United States)

Markó, Lajos; Molnár, Gergo Attila; Wagner, Zoltán; Koszegi, Tamás; Matus, Zoltán; Mohás, Márton; Kuzma, Mónika; Szijártó, István András; Wittmann, István

2008-01-13

Evaluation study, the rate of microalbuminuria positivity among the immunonephelometrically negative patients decreased to 14.5% by high performance liquid chromatography and the decrease in the number of microalbuminuria positive cases by high performance liquid chromatography could be observed mainly in the diabetic and hypertensive group (49% vs. 7.5%), while slighter decrease could be observed in the non-diabetic hypertensive group (37% vs. 26.5%). Applying the traditional criteria, the strongest predictor was the male gender by the logistic regression analysis. In 28% of microalbuminuria negative patients by immunonephelometry the diagnosis of microalbuminuria can be established using high performance liquid chromatography. Almost in one-third of microalbuminuria negative patients by immunonephelometry the diagnosis of microalbuminuria can be established by high performance liquid chromatography for which diagnosis three constitutive urine examinations are still needed. New criteria determined by the Heart Outcomes Prevention Evaluation study can be used neither in case of diabetic and hypertensive patients, nor in the case of non-diabetic hypertensive patients. The gender as the most important predictor of microalbuminuria cannot be ignored.

Establishment of analysis method for methane detection by gas chromatography

Science.gov (United States)

Liu, Xinyuan; Yang, Jie; Ye, Tianyi; Han, Zeyu

2018-02-01

The study focused on the establishment of analysis method for methane determination by gas chromatography. Methane was detected by hydrogen flame ionization detector, and the quantitative relationship was determined by working curve of y=2041.2x+2187 with correlation coefficient of 0.9979. The relative standard deviation of 2.60-6.33% and the recovery rate of 96.36%∼105.89% were obtained during the parallel determination of standard gas. This method was not quite suitable for biogas content analysis because methane content in biogas would be over the measurement range in this method.

Optimizing separations in online comprehensive two‐dimensional liquid chromatography

OpenAIRE

Pirok, Bob W.J.; Gargano, Andrea F.G.; Schoenmakers, Peter J.

2017-01-01

Abstract Online comprehensive two‐dimensional liquid chromatography has become an attractive option for the analysis of complex nonvolatile samples found in various fields (e.g. environmental studies, food, life, and polymer sciences). Two‐dimensional liquid chromatography complements the highly popular hyphenated systems that combine liquid chromatography with mass spectrometry. Two‐dimensional liquid chromatography is also applied to the analysis of samples that are not compatible with mass...

South Aegean volcanic glass. Separation and analysis by INAA and EPMA

International Nuclear Information System (INIS)

Saminger, S.; Peltz, C.; Bichler, M.

2000-01-01

Pumice from the major volcanic sources (Milos, Nisyros, Yali, Kos and Santorini) in the South Aegean region was investigated to reveal the differences between the composition of the bulk material, which contains a certain percentage of crystallites, and the pure glass phase, which is the main constituent. The knowledge of these differences is important for the identification of vitric tephra layers found in the Eastern Mediterranean region in archaeological context, in deep sea drilling cores and lake sediments. Eruption products, deposited at some distance, show not only a decrease in their grain size, but also have usually lost their crystalline fraction due to gravity separation and consist only of glass shards. Major element distributions in such layers and in pumiceous glass are not sufficient for a reliable identification of the volcanic source, as several eruptions are known to have produced chemically very similar tephra layers in this region. Trace element data, especially of the rather immobile rare earth elements (REEs), can provide greater information on tephra originating from different volcanic eruptions. Therefore, a technique has been developed to separate the glass phase from different primary pumices to reveal differences in their trace element distributions. The concentrations of the major constituents, in particular Al, Ca, Fe, Mg, Mn, Na, Si, and Ti were determined by electron probe microanalysis (EPMA), those of Al, As, Ba, Ca, Ce, Co, Cr, Cs, Dy, Eu, Fe, Hf, K, La, Lu, Mn, Na, Nd, Rb, Sb, Sc, Sm, Ta, Th, Ti, U, V, Yb and Zr by instrumental neutron activation analysis. Subtle differences between the compositions of the glass phase and the bulk material are explained by differentiation during partial crystallization. Their applicability to the classification of tephra layers is demonstrated. (author)

Ion chromatography for the precise analysis of chloride and sodium in sweat for the diagnosis of cystic fibrosis

NARCIS (Netherlands)

Doorn, J.; Storteboom, T. T. R.; Mulder, A. M.; de Jong, W. H. A.; Rottier, B. L.; Kema, I. P.

BACKGROUND: Measurement of chloride in sweat is an essential part of the diagnostic algorithm for cystic fibrosis. The lack in sensitivity and reproducibility of current methods led us to develop an ion chromatography/high-performance liquid chromatography (IC/HPLC) method, suitable for the analysis

Quantitative analysis of crystalline and remaining glass phases in CaO-B2O3-SiO2 ternary system glass ceramics

International Nuclear Information System (INIS)

He Ming; Wu Mengqiang; Zhang Shuren; Zhou Xiaohua; Zhang Ting; Chen Song

2010-01-01

Research highlights: → As for CBS ternary system glass ceramics, due to the complex phase compositions, many methods could be difficult to determine quantitatively the absolute amounts of crystalline and remaining oxides. In this study, an available method based on the Rietveld method was used to quantitatively analyze the relative weight fraction and densities of crystalline phases. These above data are used to obtain a table of both relative weight fraction of crystalline phases and densities of all phases including CBS LTCC. Using volume additivity rule, it is possible to analysis quantitatively the absolute weight fraction of crystalline phases and also the oxides molar content in the remaining glass. - Abstract: Based on Rietveld method of X-ray techniques and volume additivity rule, a new method was developed to quantitatively analyze the phase composition of CaO-B 2 O 3 -SiO 2 ternary system glass ceramics. Lattice parameters, densities and relative weight fractions of crystalline phases in CaO-B 2 O 3 -SiO 2 ternary system were obtained by X-ray diffraction (XRD) refinement. According to the relative weight fraction of crystalline phases and densities of various components, the volume additivity rule was revealed by calculating the absolute weight fraction of crystalline phases of CaO-B 2 O 3 -SiO 2 glass ceramics. In addition, molar contents of the oxides in the remaining glass can also be determined by this method. Comparing this method with internal standard method, it is found that the maximum deviations of the crystallinity and the absolute weight fraction of crystalline phases are less than 2.6% and 2.9%, respectively. As a result, quantitative evaluation of CaO-B 2 O 3 -SiO 2 ternary system glass ceramics can be achieved using this method.

Gas Chromatography-Mass Spectroscopic (GC-MS) Analysis of n ...

African Journals Online (AJOL)

tuber-regium (synonym Pleurotus tuber regium) using gas chromatography-mass spectroscopic (GC-. MS) techniques. Methods: The n-hexane extract of the sclerotia ... Soxhlet extraction and analysed using gas chromatography-mass spectroscopic (MS) techniques. ..... Phytochemical composition of Pleurotus tuber regium.

Predicting bioactive glass properties from the molecular chemical composition: glass transition temperature.

Science.gov (United States)

O'Donnell, Matthew D

2011-05-01

The glass transition temperature (T(g)) of inorganic glasses is an important parameter than can be used to correlate with other glass properties, such as dissolution rate, which governs in vitro and in vivo bioactivity. Seven bioactive glass compositional series reported in the literature (77 in total) were analysed here with T(g) values obtained by a number of different methods: differential thermal analysis, differential scanning calorimetry and dilatometry. An iterative least-squares fitting method was used to correlate T(g) from thermal analysis of these compositions with the levels of individual oxide and fluoride components in the glasses. When all seven series were fitted a reasonable correlation was found between calculated and experimental values (R(2)=0.89). When the two compositional series that were designed in weight percentages (the remaining five were designed in molar percentage) were removed from the model an improved fit was achieved (R(2)=0.97). This study shows that T(g) for a wide range in compositions (e.g. SiO(2) content of 37.3-68.4 mol.%) can be predicted to reasonable accuracy enabling processing parameters to be predicted such as annealing, fibre-drawing and sintering temperatures. Copyright © 2011 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

Quantitative Analysis of Tetramethylenedisulfotetramine ("Tetramine") Spiked into Beverages by Liquid Chromatography Tandem Mass Spectrometry with Validation by Gas Chromatography Mass Spectrometry

Energy Technology Data Exchange (ETDEWEB)

Owens, J; Hok, S; Alcaraz, A; Koester, C

2008-11-13

Tetramethylenedisulfotetramine, commonly known as tetramine, is a highly neurotoxic rodenticide (human oral LD{sub 50} = 0.1 mg/kg) used in hundreds of deliberate food poisoning events in China. Here we describe a method for quantitation of tetramine spiked into beverages, including milk, juice, tea, cola, and water and cleaned up by C8 solid phase extraction and liquid-liquid extraction. Quantitation by high performance liquid chromatography tandem mass spectrometry (LC/MS/MS) was based upon fragmentation of m/z 347 to m/z 268. The method was validated by gas chromatography mass spectrometry (GC/MS) operated in SIM mode for ions m/z 212, 240, and 360. The limit of quantitation was 0.10 {micro}g/mL by LC/MS/MS versus 0.15 {micro}g/mL for GC/MS. Fortifications of the beverages at 2.5 {micro}g/mL and 0.25 {micro}g/mL were recovered ranging from 73-128% by liquid-liquid extraction for GC/MS analysis, 13-96% by SPE and 10-101% by liquid-liquid extraction for LC/MS/MS analysis.

Quantitative Analysis of Tetramethylenedisulfotetramine ('Tetramine') Spiked into Beverages by Liquid Chromatography Tandem Mass Spectrometry with Validation by Gas Chromatography Mass Spectrometry

International Nuclear Information System (INIS)

Owens, J.; Hok, S.; Alcaraz, A.; Koester, C.

2008-01-01

Tetramethylenedisulfotetramine, commonly known as tetramine, is a highly neurotoxic rodenticide (human oral LD 50 = 0.1 mg/kg) used in hundreds of deliberate food poisoning events in China. Here we describe a method for quantitation of tetramine spiked into beverages, including milk, juice, tea, cola, and water and cleaned up by C8 solid phase extraction and liquid-liquid extraction. Quantitation by high performance liquid chromatography tandem mass spectrometry (LC/MS/MS) was based upon fragmentation of m/z 347 to m/z 268. The method was validated by gas chromatography mass spectrometry (GC/MS) operated in SIM mode for ions m/z 212, 240, and 360. The limit of quantitation was 0.10 (micro)g/mL by LC/MS/MS versus 0.15 (micro)g/mL for GC/MS. Fortifications of the beverages at 2.5 (micro)g/mL and 0.25 (micro)g/mL were recovered ranging from 73-128% by liquid-liquid extraction for GC/MS analysis, 13-96% by SPE and 10-101% by liquid-liquid extraction for LC/MS/MS analysis.

Analysis of radioactive mixed hazardous waste using derivatization gas chromatography/mass spectrometry, liquid chromatography, and liquid chromatography/mass spectrometry

International Nuclear Information System (INIS)

Campbell, J.A.; Lerner, B.D.; Bean, R.M.; Grant, K.E.; Lucke, R.B.; Mong, G.M.; Clauss, S.A.

1994-08-01

Six samples of core segments from Tank 101-SY were analyzed for chelators, chelator fragments, and several carboxylic acids by derivatization gas chromatography/mass spectrometry. The major components detected were ethylenediaminetetraacetic acid, nitroso-iminodiacetic acid, nitrilotriacetic acid, citric acid, succinic acid, and ethylenediaminetriacetic acid. The chelator of highest concentration was ethylenediaminetetraacetic acid in all six samples analyzed. Liquid chromatography was used to quantitate low molecular weight acids including oxalic, formic, glycolic, and acetic acids, which are present in the waste as acid salts. From 23 to 61% of the total organic carbon in the samples analyzed was accounted for by these acids

Optimizing separations in online comprehensive two‐dimensional liquid chromatography

Science.gov (United States)

Gargano, Andrea F.G.; Schoenmakers, Peter J.

2017-01-01

Abstract Online comprehensive two‐dimensional liquid chromatography has become an attractive option for the analysis of complex nonvolatile samples found in various fields (e.g. environmental studies, food, life, and polymer sciences). Two‐dimensional liquid chromatography complements the highly popular hyphenated systems that combine liquid chromatography with mass spectrometry. Two‐dimensional liquid chromatography is also applied to the analysis of samples that are not compatible with mass spectrometry (e.g. high‐molecular‐weight polymers), providing important information on the distribution of the sample components along chemical dimensions (molecular weight, charge, lipophilicity, stereochemistry, etc.). Also, in comparison with conventional one‐dimensional liquid chromatography, two‐dimensional liquid chromatography provides a greater separation power (peak capacity). Because of the additional selectivity and higher peak capacity, the combination of two‐dimensional liquid chromatography with mass spectrometry allows for simpler mixtures of compounds to be introduced in the ion source at any given time, improving quantitative analysis by reducing matrix effects. In this review, we summarize the rationale and principles of two‐dimensional liquid chromatography experiments, describe advantages and disadvantages of combining different selectivities and discuss strategies to improve the quality of two‐dimensional liquid chromatography separations. PMID:29027363

Study on Surface Modification of Glass Bead by a Block Copolymer Coupling Agent

Institute of Scientific and Technical Information of China (English)

LI Yin; ZHANG Bing; ZHOU Xiao-dong

2008-01-01

A tri-block copolymer coupling agent polystyrene biock-poly(n-butyl-acrylate)-block-poly(r-methacryloxypro pylt rimethoxysilane)(PS-b-PnBA-b-PMPS)was synthesized by atom transfer radical polymerization(ATRP),and its molecular structure was characterized by fourier-transform infrared spectra,hydrogen nuclear magnetic resonance and gel permeation chromatography.The glass bead was treated with the block copolymer coupling agent,and then studied by transmission electron microscopy.The result showed that strong interaction was formed between the block copolymer coupling agent and the surface of glass bead,and then the block of poly(n-butylacrylate)formed a layer of film on the surface.

Capillary column switching restricted-access media-liquid chromatography-electrospray ionization-tandem mass spectrometry system for simultaneous and direct analysis of drugs in biofluids.

Science.gov (United States)

Santos-Neto, Alvaro J; Markides, Karin E; Sjöberg, Per J R; Bergquist, Jonas; Lancas, Fernando M

2007-08-15

Capillary online restricted-access media-liquid chromatography-electrospray ionization-tandem mass spectrometry (RAM-LC-ESI-MS/MS) for direct analysis of drugs and metabolites spiked in biological fluids was developed. Using a column switching setup it was possible to perform effective sample preparation and analysis of raw biological fluids (plasma and urine) without matrix effects in the electrospray mass spectrometric detection step. The peak focusing efficiency of the extraction column was more effective in backflush compared to foreflush mode. The system was able to concentrate diminished samples of polar drugs and their metabolites reaching quantifiable results as low as 1 ng/mL utilizing a sample volume of only 333 nL of biofluids. New column hardware was developed to circumvent clogging problems experienced with plasma injections. The glass fiber filter frit, which is commonly used, was replaced with a short piece of 20 microm i.d. fused silica capillary. The extraction columns were able to handle up to 60 injections and showed a high loading capacity, making the saturation of the MS detector the limiting factor on the linear dynamic range. The simultaneous separation and detection of 10 drugs and metabolites was obtained in 8 min of analysis, including the online sample preparation and enrichment step.

Polymorphic crystallization of metal-metalloid-glasses above the glass transition temperature

International Nuclear Information System (INIS)

Koster, U.; Schunemann, U.; Stephenson, G.B.; Brauer, S.; Sutton, M.

1992-01-01

Crystallization of metal-metalloid glasses is known to proceed by nucleation and growth processes. Using crystallization statistics in partially crystallized glasses, at temperatures below the glass transition temperature, time-dependent heterogeneous nucleation has been found to occur at a number of quenched-in nucleation sites. Close to the glass transition temperature crystallization proceeds so rapidly that partially crystallized microstructures could not be obtained. Initial results form fully crystallized glasses exhibit evidence for a transient homogeneous nucleation process at higher temperatures. These conclusions are derived post mortem. At there may be some change of the microstructure after crystallization is finished or during he subsequent quenching, it is desirable to directly obtain information during the early stages of crystallization. Recently reported work by Sutton et al. showed that structural changes can be observed in situ during crystallization by time-resolved x-ray diffraction on time scales as short as milliseconds. The aim o the paper is to present the authors study of the crystallization behavior at temperatures near the glass transition by in-situ x-ray diffraction studies and by microstructural analysis after rapid heating experiments. The results are compared to those derived from a computer model of the crystallization process

Analysis of cracking in glass molds made of cast iron

Science.gov (United States)

Leushin, I. O.; Chistyakov, D. G.

2014-09-01

The cracking in the parts of cast iron molds intended for glass is considered, and this cracking substantially affects the operation of glass-blowing equipment, maintainability, and the replacement of mold sets. The processes that cause cracking in the parts of glass molds and initiate crack growth are studied.

Chromatography.

Science.gov (United States)

Brantley, L. Reed, Sr.; Demanche, Edna L.; Klemm, E. Barbara; Kyselka, Will; Phillips, Edwin A.; Pottenger, Francis M.; Yamamoto, Karen N.; Young, Donald B.

This booklet presents some activities on chromatography. Directions for preparing leaf pigment extracts using alcohol are given, and paper chromatography and thin-layer chromatography are described as modifications of the basic principles of chromatography. (KHR)

Structural and optical properties of antimony-germanate-borate glass and glass fiber co-doped Eu3+ and Ag nanoparticles.

Science.gov (United States)

Zmojda, Jacek; Kochanowicz, Marcin; Miluski, Piotr; Baranowska, Agata; Pisarski, Wojciech A; Pisarska, Joanna; Jadach, Renata; Sitarz, Maciej; Dorosz, Dominik

2018-08-05

In the paper analysis of structural and luminescent properties of antimony-germanate-borate glasses and glass fiber co-doped with 0.6AgNO 3 /0.2Eu 2 O 3 are presented. Heat treatment of the fabricated glass and optical fiber (400 °C, 12 h) enabled to obtain Ag nanoparticles (NPs) with average size 30-50 nm on their surface. It has been proofed that silver ions migrate to the glass surface, where they are reduced to Ag 0 nanoparticles. Simultaneously, FTIR analysis showed that heat treatment of the glass and optical fiber increases the local symmetry of the Eu 3+ site. Copyright © 2018 Elsevier B.V. All rights reserved.

Glass consistency and glass performance

International Nuclear Information System (INIS)

Plodinec, M.J.; Ramsey, W.G.

1994-01-01

Glass produced by the Defense Waste Processing Facility (DWPF) will have to consistently be more durable than a benchmark glass (evaluated using a short-term leach test), with high confidence. The DWPF has developed a Glass Product Control Program to comply with this specification. However, it is not clear what relevance product consistency has on long-term glass performance. In this report, the authors show that DWPF glass, produced in compliance with this specification, can be expected to effectively limit the release of soluble radionuclides to natural environments. However, the release of insoluble radionuclides to the environment will be limited by their solubility, and not glass durability

Geochemical characterization of impact glasses from the Zhamanshin crater by various modes of activation analysis. Remarks on genesis of irghizites

International Nuclear Information System (INIS)

Mizera, J.; Academy of Sciences of the Czech Republic, Prague; Randa, Z.; Tomandl, I.

2012-01-01

A large set of impact glasses from the Zhamanshin crater in Kazakhstan was analyzed by various modes of instrumental neutron activation analysis, supplemented by instrumental photon activation analysis and prompt gamma-ray activation analysis. Results of the determination of more than forty major and trace elements have shown that the analyzed set of homogeneous, tektite-like impact glasses with size of several centimeters and of various forms could be divided into two geochemically different groups. The lustrous, silica rich (acidic) glasses with high Ni content have been classified conventionally as irghizites. The dull, silica poor (basic) glasses with very low Ni content should not be confused with the large, heterogeneous impactite forms-zhamanshinites, but considered as a separate type of impact glass. Within both primary groups, further division has been suggested based on lower contents of Ni in an irghizite subgroup, and evidence of mixing of source materials for both primary groups in a part of the basic glasses. Based on the contents of Ni, Cr, Mn, Fe and Co, an ordinary chondrite impactor has been suggested with its contribution to the irghizite matter ranging between 4 and 21%. Possible source materials and impact processes leading to irghizite formation have been outlined. (author)

Supercritical fluid chromatography in drug analysis: a literature survey.

Science.gov (United States)

Salvador, A; Jaime, M A; Becerra, G; Guardia, M de L

1996-08-01

The applications of supercritical fluid chromatography to the analysis of drugs have been carefully revised from the literature compiled in the Analytical Abstracts until March 1994. Easy-to-read tables provide useful information about the state-of-the-art and possibilities offered by SFC in pharmaceutical analysis. The tables comprise extensive data about samples analyzed, pharmaceutical principles determined, solvents used and sample quantity injected, supercritical fluids and modifiers employed, injection system, instrumentation, experimental conditions for chromatographic separations (density, pressure, flow, temperature), characteristics of columns employed (type, support, length, diameter, particle film thickness, stationary phase), detectors, type of restrictors, and also some analytical features of the methods developed (such as retention time, resolution, sensitivity, limit of detection and relative standard deviation).

Electrical properties of phosphate glasses

International Nuclear Information System (INIS)

Mogus-Milankovic, A; Santic, A; Reis, S T; Day, D E

2009-01-01

Investigation of the electrical properties of phosphate glasses where transition metal oxide such as iron oxide is the network former and network modifier is presented. Phosphate glasses containing iron are electronically conducting glasses where the polaronic conduction is due to the electron hopping from low to high iron valence state. The identification of structural defects caused by ion/polaron migration, the analysis of dipolar states and electrical conductivity in iron phosphate glasses containing various alkali and mixed alkali ions was performed on the basis of the impedance spectroscopy (IS). The changes in electrical conductivity from as-quenched phosphate glass to fully crystallized glass (glass-ceramics) by IS are analyzed. A change in the characteristic features of IS follows the changes in glass and crystallized glass network. Using IS, the contribution of glass matrix, crystallized grains and grain boundary to the total electrical conductivity for iron phosphate glasses was analyzed. It was shown that decrease in conductivity is caused by discontinuities in the conduction pathways as a result of the disruption of crystalline network where two or more crystalline phases are formed. Also, phosphate-based glasses offer a unique range of biomaterials, as they form direct chemical bonding with hard/soft tissue. The surface charges of bioactive glasses are recognized to be the most important factors in determining biological responses. The improved bioactivity of the bioactive glasses as a result of the effects of the surface charges generated by electrical polarization is discussed.

High-Throughput Analysis of Sucrose Fatty Acid Esters by Supercritical Fluid Chromatography/Tandem Mass Spectrometry

Science.gov (United States)

Hori, Katsuhito; Tsumura, Kazunobu; Fukusaki, Eiichiro; Bamba, Takeshi

2014-01-01

Supercritical fluid chromatography (SFC) coupled with triple quadrupole mass spectrometry was applied to the profiling of sucrose fatty acid esters (SEs). The SFC conditions (column and modifier gradient) were optimized for the effective separation of SEs. In the column test, a silica gel reversed-phase column was selected. Then, the method was used for the detailed characterization of commercial SEs and the successful analysis of SEs containing different fatty acids. The present method allowed for fast and high-resolution separation of monoesters to tetra-esters within a shorter time (15 min) as compared to the conventional high-performance liquid chromatography. The applicability of our method for the analysis of SEs was thus demonstrated. PMID:26819875

Crystal growth in zinc borosilicate glasses

Science.gov (United States)

Kullberg, Ana T. G.; Lopes, Andreia A. S.; Veiga, João P. B.; Monteiro, Regina C. C.

2017-01-01

Glass samples with a molar composition (64+x)ZnO-(16-x)B2O3-20SiO2, where x=0 or 1, were successfully synthesized using a melt-quenching technique. Based on differential thermal analysis data, the produced glass samples were submitted to controlled heat-treatments at selected temperatures (610, 615 and 620 °C) during various times ranging from 8 to 30 h. The crystallization of willemite (Zn2SiO4) within the glass matrix was confirmed by means of X-ray diffraction (XRD) and scanning electron microscopy (SEM). Under specific heat-treatment conditions, transparent nanocomposite glass-ceramics were obtained, as confirmed by UV-vis spectroscopy. The influence of temperature, holding time and glass composition on crystal growth was investigated. The mean crystallite size was determined by image analysis on SEM micrographs. The results indicated an increase on the crystallite size and density with time and temperature. The change of crystallite size with time for the heat-treatments at 615 and 620 °C depended on the glass composition. Under fixed heat-treatment conditions, the crystallite density was comparatively higher for the glass composition with higher ZnO content.

Analysis of soda-lime glasses using non-negative matrix factor deconvolution of Raman spectra

OpenAIRE

Woelffel , William; Claireaux , Corinne; Toplis , Michael J.; Burov , Ekaterina; Barthel , Etienne; Shukla , Abhay; Biscaras , Johan; Chopinet , Marie-Hélène; Gouillart , Emmanuelle

2015-01-01

International audience; Novel statistical analysis and machine learning algorithms are proposed for the deconvolution and interpretation of Raman spectra of silicate glasses in the Na 2 O-CaO-SiO 2 system. Raman spectra are acquired along diffusion profiles of three pairs of glasses centered around an average composition of 69. 9 wt. % SiO 2 , 12. 7 wt. % CaO , 16. 8 wt. % Na 2 O. The shape changes of the Raman spectra across the compositional domain are analyzed using a combination of princi...

Copper oxide content dependence of crystallization behavior, glass forming ability, glass stability and fragility of lithium borate glasses

International Nuclear Information System (INIS)

Soliman, A.A.; Kashif, I.

2010-01-01

Differential thermal analysis (DTA) and X-ray diffraction (XRD) have been employed to investigate the copper oxide content dependence of the glass transition temperatures data, activation energy for the glass transition E t , glass stability GS, fragility index Fi, the glass-forming ability (GFA) and crystallization behavior of {(100-x) mol% Li 2 B 4 O 7 -x mol% CuO} glass samples, where x=0-40 mol% CuO. From the dependence of the glass transition temperature T g on the heating rate β, the fragility, F i , and the activation energy, E t , have been calculated. It is seen that F i and E t are attained their minimum values at 0 x -T g , SCL region and the GS. The GFA has been investigated on the basis of Hruby parameter K H , which is a strong indicator of GFA, and the relaxation time. Results of GFA are in good agreement with the fragility index, F i , calculations indicating that {90Li 2 B 4 O 7 .10CuO} is the best glass former. The stronger glass forming ability has decreasing the fragility index. XRD result indicates that no fully amorphous samples but a mixture of crystalline and amorphous phases are formed in the samples containing x>25 mol% CuO and below it composed of glassy phase. Increasing the CuO content above 25 mol% helps the crystallization process, and thus promotes a distinct SCL region. XRD suggests the presence of micro-crystallites of remaining residual amorphous matrix by increasing the CuO content.

Some recent developments in spin glasses

Indian Academy of Sciences (India)

I give some experimental and theoretical background to spin glasses, and then discuss the nature of the phase transition in spin glasses with vector spins. Results of Monte Carlo simulations of the Heisenberg spin glass model in three dimensions are presented. A finite-size scaling analysis of the correlation length of the ...

The application of energy-dispersive X-Ray fluorescence spectrometry (EDXRF) to the analysis of ceramic glasses

International Nuclear Information System (INIS)

Ben Abdelwahed, Haifa; Reguigui, Nafaa; Ghdira, Lotfi; Khosrof, S.

2005-01-01

The measurement of energies and intensities of fluorescent X-rays emitted from a given material when atoms are bombarded with suitable projectiles like electrons, protons, α particles or photons has been successfully used for non-destructive elemental analysis in many applications, especially in the analysis of ceramic glasses. Use of radioisotopes as a source of excitation radiation in combination with high resolution semiconductor detectors in x-ray fluorescence has found wide applications in elemental analysis. A radioisotope excited X-ray fluorescence spectrometer consisting of a standard 5.45mm Si(Li) detector having a resolution of 200 eV at 5.9 keV coupled to a TRUMP-8K multichannel analyzer has been used. Tow sources of annular geometry using 10 mCi 109Cd and 10 mCi 55Fe together with PC AXIL software have been used for this study of tile-pavement glasses of ''Ksar Said'' in Tunisia. Analytical data shows that those tile pavement witch are broken in the 19th century from France (Marseille) have not the same composition of Tunisian tile pavement. Referring to our data, The kind of that analyzed glasses is of alkaline lead. we found also, through this study, the elemental compositions of different pigments (green, blue, brownish, yellow, white and red) used to color that tile-pavement glasses

The application of energy-dispersive X-Ray Fluorescence spectrometry (EDXRF) to the analysis of ceramic glasses

International Nuclear Information System (INIS)

Ben Abdelwahed, H.; Reguigui, N.; Ghidira, L.; Khosrof, S.

2005-01-01

The measurement of energies and intensities of fluorescent X-rays emitted from a given material when atoms are bombarded with suitable projectiles like electrons, protons,α particles or photons have been successfully used for non destructive elemental analysis in many applications, especially in the analysis of ceramic glasses. Use of radioisotopes as a source of excitation radiation in combination with high resolution semiconductor detectors in x-ray fluorescence has found wide applications in elemental analysis. A radioisotope excited X-ray fluorescence spectrometer consisting of a standard 5.45mm Si(Li) detector having a resolution of 200 eV at 5.9 KeV coupled to a TRUMP -8K multichannel analyser has been used. Two sources of annular geometry using 10 mCi 109 CD and 10 mCi 55 Fe together with PC AXIL software have been used for this study of tile-pavement glasses of ''Ksar Said'' in Tunisia. Analytical data shows that those tile pavements which are broken in the 19th century from France (Marseille) have not the same composition of Tunisian tile pavement. Referring to our data, the kind of that analysed glasses is of alkaline lead. We found also, through this study, the elemental compositions of different pigments (green, blue, brownish, yellow, white and red) used to color those tile-pavement glasses

Chemical analysis of simulated high level waste glasses to support stage III sulfate solubility modeling

Energy Technology Data Exchange (ETDEWEB)

Fox, K. M. [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL)

2016-03-17

The U.S. Department of Energy (DOE), Office of Environmental Management (EM) is sponsoring an international, collaborative project to develop a fundamental model for sulfate solubility in nuclear waste glass. The solubility of sulfate has a significant impact on the achievable waste loading for nuclear waste forms within the DOE complex. These wastes can contain relatively high concentrations of sulfate, which has low solubility in borosilicate glass. This is a significant issue for low-activity waste (LAW) glass and is projected to have a major impact on the Hanford Tank Waste Treatment and Immobilization Plant (WTP). Sulfate solubility has also been a limiting factor for recent high level waste (HLW) sludge processed at the Savannah River Site (SRS) Defense Waste Processing Facility (DWPF). The low solubility of sulfate in glass, along with melter and off-gas corrosion constraints, dictate that the waste be blended with lower sulfate concentration waste sources or washed to remove sulfate prior to vitrification. The development of enhanced borosilicate glass compositions with improved sulfate solubility will allow for higher waste loadings and accelerate mission completion.The objective of the current scope being pursued by SHU is to mature the sulfate solubility model to the point where it can be used to guide glass composition development for DWPF and WTP, allowing for enhanced waste loadings and waste throughput at these facilities. A series of targeted glass compositions was selected to resolve data gaps in the model and is identified as Stage III. SHU fabricated these glasses and sent samples to SRNL for chemical composition analysis. SHU will use the resulting data to enhance the sulfate solubility model and resolve any deficiencies. In this report, SRNL provides chemical analyses for the Stage III, simulated HLW glasses fabricated by SHU in support of the sulfate solubility model development.

Measurement of the volatility and glass transition temperatures of glasses produced during the DWPF startup test program

International Nuclear Information System (INIS)

Marra, J.C.; Harbour, J.R.

1995-01-01

The Defense Waste Processing Facility (DWPF) will immobilize high-level radioactive waste currently stored in underground tanks at the Savannah River Site by incorporating the waste into a glass matrix. The molten waste glass will be poured into stainless steel canisters which will be welded shut to produce the final waste form. One specification requires that any volatiles produced as a result of accidentally heating the waste glass to the glass transition temperature be identified. Glass samples from five melter campaigns, run as part of the DWPF Startup Test Program, were analyzed to determine glass transition temperatures and to examine the volatilization (by weight loss). Glass transition temperatures (T g ) for the glasses, determined by differential scanning calorimetry (DSC), ranged between 445 C and 474 C. Thermogravimetric analysis (TGA) scans showed that no overall weight loss occurred in any of the glass samples when heated to 500 C. Therefore, no volatility will occur in the final glass product when heated up to 500 C

Analysis of the hologram recording on the novel chloride photo-thermo-refractive glass

Science.gov (United States)

Ivanov, S. A.; Nikonorov, N. V.; Dubrovin, V. D.; Krykova, V. A.

2017-05-01

In this research, we present new holographic material based on fluoride photo-thermo-refractive glass(PTR) - chloride PTR glass. One of the benefit of this type of PTR glass is positive refractive index change. During this work, for the first-time volume Bragg gratings were recorded in this kind of material. The first experiments revealed that such gratings are mixed i.e. possess both absorption and phase components. Complex analysis shows that both refractive index and absorption coefficient are modulated inside the grating structure. We found out that at first there is no strict dependence of the refractive index change from dosage, but as we continue the process of thermal treatment - dependence is appear. Exposure influence on the refractive index change for this glass differs from fluoride one and shows some sort of saturation after the exposure of 4-6 J/cm2 . We distinguished refractive index change and absorption coefficient change and observed both behavior with increasing thermal treatment time. We found out that the increase of thermal treatment time results in the significant refractive index change. At the same time the absorption does `not practically change. It was found that maximum modulation of refractive index is comparable with fluoride PTR glass and achieves value of 1600 ppm. The modulation of absorption is equal to induced absorption caused by silver nanoparticles and depends from reading wavelength. Our study shows that almost all absorption is modulated inside the grating.

Evaluation of three gas chromatography and two direct mass spectrometry techniques for aroma analysis of dried red bell peppers

NARCIS (Netherlands)

Ruth, van S.M.; Boscaini, E.; Mayr, D.; Pugh, J.; Posthumus, M.A.

2003-01-01

Three gas chromatography methods and two direct mass spectrometry techniques were compared for the analysis of the aroma of rehydrated diced red bell peppers. Gas chromatography methods included systems with olfactometry detection (GC-O), flame ionisation detection (GC-FID) and mass spectrometry

Supercritical fluid chromatography

Science.gov (United States)

Vigdergauz, M. S.; Lobachev, A. L.; Lobacheva, I. V.; Platonov, I. A.

1992-03-01

The characteristic features of supercritical fluid chromatography (SCFC) are examined and there is a brief historical note concerning the development of the method. Information concerning the use of supercritical fluid chromatography in the analysis of objects of different nature is presented in the form of a table. The roles of the mobile and stationary phases in the separation process and the characteristic features of the apparatus and of the use of the method in physicochemical research are discussed. The bibliography includes 364 references.

Float glass innovation in the flat glass industry

CERN Document Server

Uusitalo, Olavi

2014-01-01

A thorough industry analysis is of utmost importance for a study on the impact of technological changes on industry structure. This book evaluates the consequences of a vaguely chosen level of an industry analysis. Too broad a definition of the industry may disaggregate sub-industries, processing industries and international aspects. This is illustrated by revisiting an industry study upon which the dominant design model was based. Readers will see and understand the consequences of too broadly defined industries together with quantitative research approach can have. The book argues that the nature of the industry should define the level of the analysis. This is done by revisiting the flat glass industry study, on which Anderson and Tushman’s (1990) dominant design model is partly based. In their study Anderson and Tushman defined the flat glass industry based on four-digit SIC codes. It is argued that this definition was too broad and it disaggregated important sub-industries, processing industries and int...

Optimizing separations in online comprehensive two-dimensional liquid chromatography.

Science.gov (United States)

Pirok, Bob W J; Gargano, Andrea F G; Schoenmakers, Peter J

2018-01-01

Online comprehensive two-dimensional liquid chromatography has become an attractive option for the analysis of complex nonvolatile samples found in various fields (e.g. environmental studies, food, life, and polymer sciences). Two-dimensional liquid chromatography complements the highly popular hyphenated systems that combine liquid chromatography with mass spectrometry. Two-dimensional liquid chromatography is also applied to the analysis of samples that are not compatible with mass spectrometry (e.g. high-molecular-weight polymers), providing important information on the distribution of the sample components along chemical dimensions (molecular weight, charge, lipophilicity, stereochemistry, etc.). Also, in comparison with conventional one-dimensional liquid chromatography, two-dimensional liquid chromatography provides a greater separation power (peak capacity). Because of the additional selectivity and higher peak capacity, the combination of two-dimensional liquid chromatography with mass spectrometry allows for simpler mixtures of compounds to be introduced in the ion source at any given time, improving quantitative analysis by reducing matrix effects. In this review, we summarize the rationale and principles of two-dimensional liquid chromatography experiments, describe advantages and disadvantages of combining different selectivities and discuss strategies to improve the quality of two-dimensional liquid chromatography separations. © 2017 The Authors. Journal of Separation Science published by WILEY-VCH Verlag GmbH & Co. KGaA.

Gas chromatography-vacuum ultraviolet spectroscopy for analysis of fatty acid methyl esters.

Science.gov (United States)

Fan, Hui; Smuts, Jonathan; Bai, Ling; Walsh, Phillip; Armstrong, Daniel W; Schug, Kevin A

2016-03-01

A new vacuum ultraviolet (VUV) detector for gas chromatography was recently developed and applied to fatty acid methyl ester (FAME) analysis. VUV detection features full spectral acquisition in a wavelength range of 115-240nm, where virtually all chemical species absorb. VUV absorption spectra of 37 FAMEs, including saturated, monounsaturated, and polyunsaturated types were recorded. Unsaturated FAMEs show significantly different gas phase absorption profiles than saturated ones, and these classes can be easily distinguished with the VUV detector. Another advantage includes differentiating cis/trans-isomeric FAMEs (e.g. oleic acid methyl ester and linoleic acid methyl ester isomers) and the ability to use VUV data analysis software for deconvolution of co-eluting signals. As a universal detector, VUV also provides high specificity, sensitivity, and a fast data acquisition rate, making it a powerful tool for fatty acid screening when combined with gas chromatography. The fatty acid profile of several food oil samples (olive, canola, vegetable, corn, sunflower and peanut oils) were analyzed in this study to demonstrate applicability to real world samples. Copyright © 2015 Elsevier Ltd. All rights reserved.

Fast and Simple Forensic Red Pen Ink Analysis Using Ultra-Performance Liquid Chromatography (UPLC)

International Nuclear Information System (INIS)

Lee, L.C.; Ying, S.L.; Wan Nur Syazwani Wan Mohamad Fuad; Ab Aziz Ishak; Khairul Osman

2016-01-01

Ultra-performance liquid chromatography (UPLC) is more effective than high performance liquid chromatography in terms of analysis speed and sensitivity. This paper presents a feasibility study on forensic red pen inks analysis using UPLC. A total of 12 varieties of red ball point pen inks were purchased from selected stationary shop. For each variety, four different individual pens were sampled to provide intra-variability within a particular variety of pen. The proposed approach is very simple that it only involved limited analysis step and chemicals. A total of 144 chromatograms were obtained from red ink entries extracted with 1.5 mL 80 % (v/v) acetonitrile. Peaks originated from pen inks were determined by comparing the chromatograms of both blank paper and blank solvent against that of ink samples. Subsequently, one-way ANOVA was conducted to discriminate all 66 possible pairs for red pen inks. Results showed that the proposed approach giving discriminating power of 95.45 %. The outcome of the study indicates that UPLC could be a fast and simple approach to red ball point pen inks analysis. (author)

UHPLC: The Greening Face of Liquid Chromatography

OpenAIRE

Cielecka-Piontek, Judyta; Zalewski, Przemys?aw; Jeli?ska, Anna; Garbacki, Piotr

2013-01-01

Pharmaceutical analysis based on chromatographic separation is an important part of studies aimed at developing routine quality analysis of drugs. High-performance liquid chromatography (HPLC) is one of the main analytical techniques recommended for drug analysis. Although it meets many criteria vital for analysis, it is time-consuming and uses a relatively high amount of organic solvents compared to other analytical techniques. Recently, Ultra-high-performance liquid chromatography (UHPLC) h...

Sinter recrystalization and properties evaluation of glass-ceramic from waste glass bottle and magnesite for extended application

Directory of Open Access Journals (Sweden)

As'mau Ibrahim Gebi

2016-12-01

Full Text Available In a bid to address environmental challenges associated with the management of waste Coca cola glass bottle, this study set out to develop glass ceramic materials using waste coca cola glass bottles and magnesite from Sakatsimta in Adamawa state. A reagent grade chrome (coloring agent were used to modify the composition of the coca cola glass bottle;  X-ray fluorescence(XRF, X-ray diffraction (XRD and Thermo gravimetric analysis (TGA were used to characterize raw materials, four batches GC-1= Coca cola glass frit +1%Cr2O3, GC-2=97% Coca cola glass frit+ 2% magnesite+1%Cr2O3, GC-3=95% Coca cola glass frit+ 4%magnesite+1%Cr2O3, GC-4=93%Coca cola glass frit+ 6%magnesite+ 1%Cr2O3 were formulated and prepared. Thermal Gradient Analysis (TGA results were used as a guide in selection of three temperatures (7000C, 7500C and 8000C used for the study, three particle sizes -106+75, -75+53, -53µm and 2 hr sintering time were also used, the sinter crystallization route of glass ceramic production was adopted. The samples were characterized by X-ray diffraction (XRD and Scanning Electron Microscope (SEM, the density, porosity, hardness and flexural strength of the resulting glass ceramics were also measured. The resulting glass ceramic materials composed mainly of wollastonite, diopside and anorthite phases depending on composition as indicated by XRD and SEM, the density of the samples increased with increasing sintering temperature and decreasing particle size. The porosity is minimal and it decreases with increasing sintering temperature and decreasing particle size. The obtained glass ceramic materials possess appreciable hardness and flexural strength with GC-3 and GC-4 having the best combination of both properties.

Thermal analysis and in vitro bioactivity of bioactive glass-alumina composites

Energy Technology Data Exchange (ETDEWEB)

Chatzistavrou, Xanthippi, E-mail: x.chatzistavrou@imperial.ac.uk [Solid State Physics Section, Physics Department, Aristotle University of Thessaloniki, 54124 Thessaloniki (Greece); Kantiranis, Nikolaos, E-mail: kantira@geo.auth.gr [School of Geology, Aristotle University of Thessaloniki, 54124 Thessaloniki (Greece); Kontonasaki, Eleana, E-mail: kont@dent.auth.gr [School of Dentistry, Department of Fixed Prosthesis and Implant Prosthodontics, Aristotle University of Thessaloniki, 54124 Thessaloniki (Greece); Chrissafis, Konstantinos, E-mail: hrisafis@physics.auth.gr [Solid State Physics Section, Physics Department, Aristotle University of Thessaloniki, 54124 Thessaloniki (Greece); Papadopoulou, Labrini, E-mail: lambrini@geo.auth.gr [School of Geology, Aristotle University of Thessaloniki, 54124 Thessaloniki (Greece); Koidis, Petros, E-mail: pkoidis@dent.auth.gr [School of Dentistry, Department of Fixed Prosthesis and Implant Prosthodontics, Aristotle University of Thessaloniki, 54124 Thessaloniki (Greece); Boccaccini, Aldo R., E-mail: a.boccaccini@imperial.ac.uk [Department of Materials, Faculty of Engineering, Imperial College, SW7 2AZ London (United Kingdom); Paraskevopoulos, Konstantinos M., E-mail: kpar@auth.gr [Solid State Physics Section, Physics Department, Aristotle University of Thessaloniki, 54124 Thessaloniki (Greece)

2011-01-15

Bioactive glass-alumina composite (BA) pellets were fabricated in the range 95/5-60/40 wt.% respectively and were heat-treated under a specific thermal treatment up to 950 {sup o}C. Control (unheated) and heat-treated pellets were immersed in Simulated Body Fluid (SBF) for bioactivity testing. All pellets before and after immersion in SBF were studied by Fourier Transform Infrared spectroscopy (FTIR), Scanning Electron Microscopy (SEM-EDS) and X-ray Diffraction (XRD) analysis. All composite pellets presented bioactive response. On the surface of the heat-treated pellets the development of a rich biological hydroxyapatite (HAp) layer was delayed for one day, compared to the respective control pellets. Independent of the proportion of the two components, all composites of each group (control and heat-treated) presented the same bioactive response as a function of immersion time in SBF. It was found that by the applied methodology, Al{sub 2}O{sub 3} can be successfully applied in bioactive glass composites without obstructing their bioactive response. - Research Highlights: {yields} Isostatically pressed glass-alumina composites presented apatite-forming ability. {yields} The interaction with SBF resulted in an aluminium phosphate phase formation. {yields} The formation of an aluminium phosphate phase enhanced the in vitro apatite growth.

Apollo 12 ropy glasses revisited

Science.gov (United States)

Wentworth, S. J.; Mckay, D. S.; Lindstrom, D. J.; Basu, A.; Martinez, R. R.; Bogard, D. D.; Garrison, D. H.

1994-01-01

We analyzed ropy glasses from Apollo 12 soils 12032 and 12033 by a variety of techniques including SEM/EDX, electron microprobe analysis, INAA, and Ar-39-Ar-40 age dating. The ropy glasses have potassium rare earth elements phosphorous (KREEP)-like compositions different from those of local Apollo 12 mare soils; it is likely that the ropy glasses are of exotic origin. Mixing calculations indicate that the ropy glasses formed from a liquid enriched in KREEP and that the ropy glass liquid also contained a significant amount of mare material. The presence of solar Ar and a trace of regolith-derived glass within the ropy glasses are evidence that the ropy glasses contain a small regolith component. Anorthosite and crystalline breccia (KREEP) clasts occur in some ropy glasses. We also found within these glasses clasts of felsite (fine-grained granitic fragments) very similar in texture and composition to the larger Apollo 12 felsites, which have a Ar-39-Ar-40 degassing age of 800 +/- 15 Ma. Measurements of 39-Ar-40-Ar in 12032 ropy glass indicate that it was degassed at the same time as the large felsite although the ropy glass was not completely degassed. The ropy glasses and felsites, therefore, probably came from the same source. Most early investigators suggested that the Apollo 12 ropy glasses were part of the ejecta deposited at the Apollo 12 site from the Copernicus impact. Our new data reinforce this model. If these ropy glasses are from Copernicus, they provide new clues to the nature of the target material at the Copernicus site, a part of the Moon that has not been sampled directly.

Core-Shell Columns in High-Performance Liquid Chromatography: Food Analysis Applications

OpenAIRE

Preti, Raffaella

2016-01-01

The increased separation efficiency provided by the new technology of column packed with core-shell particles in high-performance liquid chromatography (HPLC) has resulted in their widespread diffusion in several analytical fields: from pharmaceutical, biological, environmental, and toxicological. The present paper presents their most recent applications in food analysis. Their use has proved to be particularly advantageous for the determination of compounds at trace levels or when a large am...

Greening Reversed-Phase Liquid Chromatography Methods Using Alternative Solvents for Pharmaceutical Analysis

Directory of Open Access Journals (Sweden)

Moussa Yabré

2018-05-01

Full Text Available The greening of analytical methods has gained increasing interest in the field of pharmaceutical analysis to reduce environmental impacts and improve the health safety of analysts. Reversed-phase high-performance liquid chromatography (RP-HPLC is the most widely used analytical technique involved in pharmaceutical drug development and manufacturing, such as the quality control of bulk drugs and pharmaceutical formulations, as well as the analysis of drugs in biological samples. However, RP-HPLC methods commonly use large amounts of organic solvents and generate high quantities of waste to be disposed, leading to some issues in terms of ecological impact and operator safety. In this context, greening HPLC methods is becoming highly desirable. One strategy to reduce the impact of hazardous solvents is to replace classically used organic solvents (i.e., acetonitrile and methanol with greener ones. So far, ethanol has been the most often used alternative organic solvent. Others strategies have followed, such as the use of totally aqueous mobile phases, micellar liquid chromatography, and ionic liquids. These approaches have been well developed, as they do not require equipment investments and are rather economical. This review describes and critically discusses the recent advances in greening RP-HPLC methods dedicated to pharmaceutical analysis based on the use of alternative solvents.

Numerical study of cullet glass subjected to microwave heating and SiC susceptor effects. Part II: Exergy transfer analysis

International Nuclear Information System (INIS)

Acevedo, Luis; Usón, Sergio; Uche, Javier

2015-01-01

Highlights: • Exergy transfer analysis is proposed for the analysis of microwave glass heating. • Distribution of exergy transferred, accumulated and destroyed is quantified. • The method is applied to the comparison of different susceptor positions. - Abstract: The mathematical model of exergy transfer in cullet glass heated by microwave inside of a cubical cavity with the aid of a susceptor is presented. Part I of this paper presented a numerical combined electromagnetic and heat transfer model by applying both transient Maxwell’s equations and heat transfer equations. Then, the electromagnetic and temperature fields were used to obtain the exergy transfer analysis in the oven. Exergy transfer analysis informs us about the efficiency of energy transformations taking place during the heating process, since it explains how the quality of the energy behaves along the heating process. The rate of internal exergy, exergy flowing and destroyed exergy were obtained and presented for this transient process. Part I showed that the susceptor location could change the temperature fields of cullet glass. So, an exergy analysis is important to understand the irreversibilities produced by a susceptor during preheating (microwaves activation) and heating process of the cullet glass, and how they could be minimized. Exergy transfer analysis shows how both, electromagnetic and heat transfer, are responsible of the irreversibilities generated in the heating process

[Recent advances in analysis of petroleum geological samples by comprehensive two-dimensional gas chromatography].

Science.gov (United States)

Gao, Xuanbo; Chang, Zhenyang; Dai, Wei; Tong, Ting; Zhang, Wanfeng; He, Sheng; Zhu, Shukui

2014-10-01

Abundant geochemical information can be acquired by analyzing the chemical compositions of petroleum geological samples. The information obtained from the analysis provides scientifical evidences for petroleum exploration. However, these samples are complicated and can be easily influenced by physical (e. g. evaporation, emulsification, natural dispersion, dissolution and sorption), chemical (photodegradation) and biological (mainly microbial degradation) weathering processes. Therefore, it is very difficult to analyze the petroleum geological samples and they cannot be effectively separated by traditional gas chromatography/mass spectrometry. A newly developed separation technique, comprehensive two-dimensional gas chromatography (GC x GC), has unique advantages in complex sample analysis, and recently it has been applied to petroleum geological samples. This article mainly reviews the research progres- ses in the last five years, the main problems and the future research about GC x GC applied in the area of petroleum geology.

Thermal analysis studies of Ge additive of Se-Te glasses

International Nuclear Information System (INIS)

Mohamed, M.; Abdel-Rahim, M.A.

2016-01-01

Ge x Se 50 Te 50-x (x= 5, 15, 20, 35 at.%) bulk glasses were synthesized by the melt quenching method. The amorphous nature of the investigated glasses was determined by X-ray diffraction. Results of differential scanning calorimetry (DSC) of the studied compositions under non-isothermal conditions were reported and discussed. The glass transition temperature (T g ), onset crystallization temperature (T c ), and crystallization peak temperature (T p ) were determined from DSC traces at different heating rates. It was found that the values of T g , T c , and T p rely on both composition and heating rate. A double crystallization stages were observed in the DSC results. Various kinetics parameters such as the glass transition energy (E g ), crystallization activation energy (E c ), and rate constant (K p ) were calculated. The glass-forming ability of the studied compositions was discussed as function of the determined kinetics parameters. (orig.)

Investigation into the structure of lead-borate glass

International Nuclear Information System (INIS)

Kurtsinovskaya, R.I.

1976-01-01

X-ray phase and IR analysis of lead borate glasses show that glasses containing from 12 to 45 mole % PbO consist of several phases. A comparison of x-ray different data for lead borate and lead germanate glasses, which have two maxima on the diffraction patterns throughout the glass-formation region, shows that the microstructure of lead borate glasses is far more complex

Analysis of particulate polycyclic aromatic hydrocarbons by on-line coupled supercritical fluid extraction-liquid chromatography-gas chromatography-mass spectrometry

Science.gov (United States)

Shimmo, Masahiko; Adler, Heidi; Hyötyläinen, Tuulia; Hartonen, Kari; Kulmala, Markku; Riekkola, Marja-Liisa

An on-line supercritical fluid extraction-liquid chromatography-gas chromatography-mass spectrometry (SFE-LC-GC-MS) method was developed for the analysis of the particulate polycyclic aromatic hydrocarbons (PAHs). The limits of detection of the system for the quantification standards were in the range of 0.25-0.57 ng, while the limits of determinations for filter samples varied from 0.02 to 0.04 ng m -3 (24 h sampling). The linearity was excellent from 5 to 300 ng ( R2>0.967). The analysis could be carried out in a closed system without tedious manual sample pretreatment and with no risk of errors by contamination or loss of the analytes. The results of the SFE-LC-GC-MS method were comparable with those for Soxhlet and shake-flask extractions with GC-MS. The new method was applied to the analysis of PAHs collected by high-volume filter in the Helsinki area to study the seasonal trend of the concentrations. The individual PAH concentrations varied from 0.015 to more than 1 ng m -3, while total PAH concentrations varied from 0.81 to 5.68 ng m -3. The concentrations were generally higher in winter than in summer. The mass percentage of the total PAHs in total suspended particulates ranged from 2.85×10 -3% in July to 15.0×10 -3% in December. Increased emissions in winter, meteorological conditions, and more serious artefacts during the sampling in summer season may explain the concentration profiles.

Quantitative analysis of pharmaceuticals in biological fluids using high-performance liquid chromatography coupled to mass spectrometry: a review.

Science.gov (United States)

Plumb, R S; Dear, G J; Mallett, D N; Higton, D M; Pleasance, S; Biddlecombe, R A

2001-01-01

1. The development of bio-analysis of drug molecules over the last 10 years is reviewed, focusing on advances in sample preparation, liquid chromatography and detection. 2. Developments have led to improvements in detection sensitivity, enhancements in specificity and increased capacity. 3. Emerging technologies such as monolithic column chromatography and miniaturized chip-based systems are discussed.

Break-glass handling exceptional situations in access control

CERN Document Server

Petritsch, Helmut

2014-01-01

Helmut Petritsch describes the first holistic approach to Break-Glass which covers the whole life-cycle: from access control modeling (pre-access), to logging the security-relevant system state during Break-Glass accesses (at-access), and the automated analysis of Break-Glass accesses (post-access). Break-Glass allows users to override security restrictions in exceptional situations. While several Break-Glass models specific to given access control models have already been discussed in research (e.g., extending RBAC with Break-Glass), the author introduces a generic Break-Glass model. The pres

Nuclear microprobe analysis of carbon within glass inclusions and volcanic materials

International Nuclear Information System (INIS)

Metrich, N.; Mosbah, M.; Trocellier, P.; Clocchiatti, R.

1986-01-01

Microanalysis possibilities have been explored to determine light element concentrations within glasses (melt inclusions and basaltic glass fragments) and volcanic phenocrysts. In the first step, C was examined. The study of different spectral interferences lead to calculated detection limits of 40 μg/g for basaltic glasses and 50 μg/g for olivine crystals. The C contents of all investigated specimens range from 40 μg/g (the detection limit) to 6800 μg/g. Heterogeneities were revealed within glass inclusions. Measurements show obvious concentration profiles in basaltic glass samples. Our results agree with previous published data and are reliable. Accuracy of measurements is about 20%. 12 refs

Silicate glasses corrosion. Texture analysis of the corrosion layer

International Nuclear Information System (INIS)

Portal, Sabine

2001-01-01

We have studied the kinetic and the texture evolution of the corroded layer that forms on glass surfaces exposed to acidic solutions. The corroded layer is depleted in alkali cations and is produced by an ion exchange mechanism. It is porous and shows a lower refractive index than the one of the bulk glass. Spectroscopic ellipsometry allows determining the thickness of the layer and its refractive index. Several other techniques have been developed for characterizing the corrosion behaviour of glass surfaces: porosity is thus investigated by adsorption-desorption of nitrogen; the thickness and the composition of the layer are studied by secondary ion mass spectroscopy (S.I.M.S.); sodium concentration in the solution has been analyzed by atomic absorption. This study shows the importance of leaching conditions and glass preparation. The type of drying employed is susceptible to modify the texture and the structure of the layer. The layers produced in the early stages of the leaching process are not easily detectable. The different results lead however to the same conclusion: after a strong increase of porosity, a densification of the layer is observed with increasing time. The evolution of the layer texture could therefore modify the kinetic of the glass corrosion. (author) [fr

Analysis of small carbohydrates in several bioactive botanicals by gas chromatography with mass spectrometry and liquid chromatography with tandem mass spectrometry.

Science.gov (United States)

Moldoveanu, Serban; Scott, Wayne; Zhu, Jeff

2015-11-01

Bioactive botanicals contain natural compounds with specific biological activity, such as antibacterial, antioxidant, immune stimulating, and taste improving. A full characterization of the chemical composition of these botanicals is frequently necessary. A study of small carbohydrates from the plant materials of 18 bioactive botanicals is further described. The study presents the identification of the carbohydrate using a gas chromatographic-mass spectrometric analysis that allows detection of molecules as large as maltotetraose, after changing them into trimethylsilyl derivatives. A number of carbohydrates in the plant (fructose, glucose, mannose, sucrose, maltose, xylose, sorbitol, and myo-, chiro-, and scyllo-inositols) were quantitated using a novel liquid chromatography with tandem mass spectrometric technique. Both techniques involved new method developments. The gas chromatography with mass spectrometric analysis involved derivatization and separation on a Rxi(®)-5Sil MS column with H2 as a carrier gas. The liquid chromatographic separation was obtained using a hydrophilic interaction type column, YMC-PAC Polyamine II. The tandem mass spectrometer used an electrospray ionization source in multiple reaction monitoring positive ion mode with the detection of the adducts of the carbohydrates with Cs(+) ions. The validated quantitative procedure showed excellent precision and accuracy allowing the analysis in a wide range of concentrations of the analytes. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

DWPF GLASS BEADS AND GLASS FRIT TRANSPORT DEMONSTRATION

Energy Technology Data Exchange (ETDEWEB)

Adamson, D; Bradley Pickenheim, B

2008-11-24

DWPF is considering replacing irregularly shaped glass frit with spherical glass beads in the Slurry Mix Evaporator (SME) process to decrease the yield stress of the melter feed (a non-Newtonian Bingham Plastic). Pilot-scale testing was conducted on spherical glass beads and glass frit to determine how well the glass beads would transfer when compared to the glass frit. Process Engineering Development designed and constructed the test apparatus to aid in the understanding and impacts that spherical glass beads may have on the existing DWPF Frit Transfer System. Testing was conducted to determine if the lines would plug with the glass beads and the glass frit slurry and what is required to unplug the lines. The flow loop consisted of vertical and horizontal runs of clear PVC piping, similar in geometry to the existing system. Two different batches of glass slurry were tested: a batch of 50 wt% spherical glass beads and a batch of 50 wt% glass frit in process water. No chemicals such as formic acid was used in slurry, only water and glass formers. The glass beads used for this testing were commercially available borosilicate glass of mesh size -100+200. The glass frit was Frit 418 obtained from DWPF and is nominally -45+200 mesh. The spherical glass beads did not have a negative impact on the frit transfer system. The transferring of the spherical glass beads was much easier than the glass frit. It was difficult to create a plug with glass bead slurry in the pilot transfer system. When a small plug occurred from setting overnight with the spherical glass beads, the plug was easy to displace using only the pump. In the case of creating a man made plug in a vertical line, by filling the line with spherical glass beads and allowing the slurry to settle for days, the plug was easy to remove by using flush water. The glass frit proved to be much more difficult to transfer when compared to the spherical glass beads. The glass frit impacted the transfer system to the point

DWPF GLASS BEADS AND GLASS FRIT TRANSPORT DEMONSTRATION

International Nuclear Information System (INIS)

Adamson, D.; Pickenheim, Bradley

2008-01-01

DWPF is considering replacing irregularly shaped glass frit with spherical glass beads in the Slurry Mix Evaporator (SME) process to decrease the yield stress of the melter feed (a non-Newtonian Bingham Plastic). Pilot-scale testing was conducted on spherical glass beads and glass frit to determine how well the glass beads would transfer when compared to the glass frit. Process Engineering Development designed and constructed the test apparatus to aid in the understanding and impacts that spherical glass beads may have on the existing DWPF Frit Transfer System. Testing was conducted to determine if the lines would plug with the glass beads and the glass frit slurry and what is required to unplug the lines. The flow loop consisted of vertical and horizontal runs of clear PVC piping, similar in geometry to the existing system. Two different batches of glass slurry were tested: a batch of 50 wt% spherical glass beads and a batch of 50 wt% glass frit in process water. No chemicals such as formic acid was used in slurry, only water and glass formers. The glass beads used for this testing were commercially available borosilicate glass of mesh size -100+200. The glass frit was Frit 418 obtained from DWPF and is nominally -45+200 mesh. The spherical glass beads did not have a negative impact on the frit transfer system. The transferring of the spherical glass beads was much easier than the glass frit. It was difficult to create a plug with glass bead slurry in the pilot transfer system. When a small plug occurred from setting overnight with the spherical glass beads, the plug was easy to displace using only the pump. In the case of creating a man made plug in a vertical line, by filling the line with spherical glass beads and allowing the slurry to settle for days, the plug was easy to remove by using flush water. The glass frit proved to be much more difficult to transfer when compared to the spherical glass beads. The glass frit impacted the transfer system to the point

SEM-EDS analysis of ancient gold leaf glass mosaic tesserae. A contribution to the dating of the materials

International Nuclear Information System (INIS)

Conventi, A; Verità, M; Neri, E

2012-01-01

Metal leaf (gold, silver or their alloys) glass tesserae began to be used in wall mosaics in the first century AD (the first examples are in Rome) and their use has been uninterrupted up to day. The metal leaf could be obtained from circulating coins, jewellery or refining. According to various techniques that have changed over the centuries, the leaf was hot fixed between two glass layers. From an archaeological point of view, it is interesting to know when and where these tesserae were made, if they were new made or if they were reused tesserae recovered from earlier dismantled mosaics. The determination of the glass composition of the tesserae is not of great help in this connection, for the same kind of glass was used over long periods. Available information is still scanter for glasses produced between the 1st to 8th centuries when the batch of raw materials (a natural soda called natron and a silica-lime sand) was melted in large tank furnaces and chunks of raw glass were transported all over the Mediterranean to be remelted and shaped into manufacts in small pot furnaces. The SEM-EDS analysis is proposed in this study as a useful tool to investigate the composition of both the glass and the gold alloy in leaf tesserae from mosaics of the 1st - 9th centuries. The comparison of the composition of the gold leaf of the tesserae with that of circulating gold coins (for which an important analytical data base is available), adds further information to the glass analysis, allowing us to improve the dating of the tesserae and increase the knowledge that may result from scientific analyses. The results demonstrate that good quantitative analyses of the metal leaf can be performed and that metal leaves made of pure gold or gold-silver alloys were used.

Effect of different glasses in glass bonded zeolite

International Nuclear Information System (INIS)

Lewis, M.A.; Ackerman, J.P.; Verma, S.

1995-01-01

A mineral waste form has been developed for chloride waste salt generated during the pyrochemical treatment of spent nuclear fuel. The waste form consists of salt-occluded zeolite powders bound within a glass matrix. The zeolite contains the salt and immobilizes the fission products. The zeolite powders are hot pressed to form a mechanically stable, durable glass bonded zeolite. Further development of glass bonded zeolite as a waste form requires an understanding of the interaction between the glass and the zeolite. Properties of the glass that enhance binding and durability of the glass bonded zeolite need to be identified. Three types of glass, boroaluminosilicate, soda-lime silicate, and high silica glasses, have a range of properties and are now being investigated. Each glass was hot pressed by itself and with an equal amount of zeolite. MCC-1 leach tests were run on both. Soda-lime silicate and high silica glasses did not give a durable glass bonded zeolite. Boroaluminosilicate glasses rich in alkaline earths did bind the zeolite and gave a durable glass bonded zeolite. Scanning electron micrographs suggest that the boroaluminosilicate glasses wetted the zeolite powders better than the other glasses. Development of the glass bonded zeolite as a waste form for chloride waste salt is continuing

Simultaneous quantitative analysis of metabolites using ion-pair liquid chromatography-electrospray ionization mass spectrometry

NARCIS (Netherlands)

Coulier, L.; Bas, R.; Jespersen, S.; Verheij, E.; Werf, M.J. van der; Hankemeier, T.

2006-01-01

We have developed an analytical method, consisting of ion-pair liquid chromatography coupled to electrospray ionization mass spectrometry (IP-LC-ESI-MS), for the simultaneous quantitative analysis of several key classes of polar metabolites, like nucleotides, coenzyme A esters, sugar nucleotides,

Ionic conductivities of lithium phosphorus oxynitride glasses, polycrystals, and thin films

International Nuclear Information System (INIS)

Wang, B.; Bates, J.B.; Chakoumakos, B.C.; Sales, B.C.; Kwak, B.S.; Zuhr, R.A.; Robertson, J.D.

1994-11-01

Various lithium phosphorus oxynitrides have been prepared in the form of glasses, polycrystals, and thin films. The structures of these compounds were investigated by X-ray and neutron diffraction, X-ray photoelectron spectroscopy (XPS), and high-performance liquid chromatography (HPLC). The ac impedance measurements indicate a significant improvement of ionic conductivity as the result of incorporation of nitrogen into the structure. In the case of polycrystalline Li 2.88 PO 3.73 N 0.14 with the γ-Li 3 PO 4 structure, the conductivity increased by several orders of magnitude on small addition of nitrogen. The highest conductivities in the bulk glasses and thin films were found to be 3.0 x 10 -7 and 8.9 x 10 -7 S·cm -1 at 25 degrees C, respectively

Chemical durability of lead borosilicate glass matrix under simulated geological conditions

International Nuclear Information System (INIS)

Yalmali, Vrunda S.; Deshingkar, D.S.; Wattal, P.K.

2002-03-01

The lead borosilicate glass has been developed for vitrification of High Level Waste (HLW) stored at Trombay. This waste is contains especially high contents of sodium, uranium sulphate and iron. The glasses containing HLW are to be ultimately disposed into deep geological repositories. Long term leach rates under simulated geological conditions need to be evaluated for glass matrix. Studies were taken up to estimate the lead borosilicate glass WTR-62 matrix for chemical durability in presence of synthetic ground water. The leachant selected was based on composition of ground water sample near proposed repository site. In the first phase of these tests, the experiments were conducted for short duration of one and half month. The leaching experiments were conducted in presence of a) distilled water b) synthetic ground water c) synthetic ground water containing granite, bentonite and ferric oxide and d) synthetic ground water containing humic acid at 100 0 C. The leachate samples were analysed by pHmetry , ion chromatography and UV -VIS spectrophotometry. The normalised leach rates for lead borosilicate WTR- 62 glass matrix based on silica, boron and sulphate analyses of leachates were of the order of 10 -3 to 10 -5 gms/cm 2 /day for 45 days test period in presence of synthetic ground water as well as in presence of other materials likely to be present along with synthetic ground water. These rates are comparable to those of sodium borsilicate glass matrices reported in literature. It is known that the leach rates of glass matrix decrease with longer test durations due to formation of leached layer on its surface. The observed leach rates of lead borosilicate WTR- 62 glass matrix for 45 day tests under simulated geological conditions were found to be sufficiently encouraging to take up long term tests for evaluating its performances under repository conditions. (author)

Neutron Scattering Analysis of Water's Glass Transition and Micropore Collapse in Amorphous Solid Water.

Science.gov (United States)

Hill, Catherine R; Mitterdorfer, Christian; Youngs, Tristan G A; Bowron, Daniel T; Fraser, Helen J; Loerting, Thomas

2016-05-27

The question of the nature of water's glass transition has continued to be disputed over many years. Here we use slow heating scans (0.4  K min^{-1}) of compact amorphous solid water deposited at 77 K and an analysis of the accompanying changes in the small-angle neutron scattering signal, to study mesoscale changes in the ice network topology. From the data we infer the onset of rotational diffusion at 115 K, a sudden switchover from nondiffusive motion and enthalpy relaxation of the network at 121  K, in excellent agreement with the glass transition onset deduced from heat capacity and dielectric measurements. This indicates that water's glass transition is linked with long-range transport of water molecules on the time scale of minutes and, thus, clarifies its nature. Furthermore, the slow heating rates combined with the high crystallization resistance of the amorphous sample allow us to identify the glass transition end point at 136 K, which is well separated from the crystallization onset at 144 K-in contrast to all earlier experiments in the field.

Cordierite Glass-Ceramics for Dielectric Materials

International Nuclear Information System (INIS)

Siti Mazatul Azwa Saiyed Mohd Nurddin; Selamat, Malek; Ismail, Abdullah

2007-01-01

The objective of this project is to examine the potential of using Malaysian silica sand deposit as SiO2 raw material in producing cordierite glass-ceramics (2MgO-2Al2O3-5SiO2) for dielectric materials. Upgraded silica sands from Terengganu and ex-mining land in Perak were used in the test-works. The glass batch of the present work has a composition of 45.00% SiO2, 24.00% Al2O3, 15.00% MgO and 8.50% TiO2 as nucleation agent. From the differential thermal analysis results, the crystallization temperature was found to start around 900 deg. C. The glass samples were heat-treated at 900 deg. C and 1000 deg. C. The X-ray diffraction analysis (XRD) results showed glass-ceramics from Terengganu samples containing mainly cordierite and minor β-quartz crystals. However, glass-ceramics from ex-mining land samples contained mainly α-quartz and minor cordierite crystals. Glass-ceramics with different crystal phases exhibit different mechanical, dielectric and thermal properties. Based on the test works, both silica sand deposits, can be potentially used to produce dielectric material component

Interface mechanics and histomorphometric analysis of hydroxyapatite-coated and porous glass-ceramic implants in canine bone

DEFF Research Database (Denmark)

Nimb, L; Jensen, J S; Gotfredsen, K

1995-01-01

A canine study was performed to make a histological and biomechanical evaluation of the interface between bone and two different bioceramic implants. A newly developed glass-ceramic formed by P2O5, CaO, SiO2, and Al2O3, giving a crystal phase composed of CaP2O6-AlPO4-SiP2O7, was compared...... analysis. The ultimate shear strength for the HA-coated implants was significantly higher than in the glass-ceramic group. When these values were related to the histomorphometric measurements, the difference could be explained by the tissue-to-implant contact. The glass-ceramic showed direct contact only...... with nonmineralized, osteoid bone. The HA-coated implants, however, were integrated into the bone. The study indicated that porous glass-ceramic containing AlPO4 causes local osteomalacia and might not be suitable for clinical purposes....

Surface analysis of Borkron glass for neutron optics applications

International Nuclear Information System (INIS)

Farnoux, B.; Maaza, M.; Maaza, M.; Samuel, F.; Sella, C.

1991-01-01

Grazing Angle Neutron Reflectometry, Optical and Mechanical Roughness Profilometry techniques have been used to study the effects of the polishing operations on the surface of Borkron Schott glass (special borosilicate glass for neutron optics applications) as the polishing tool pressure P and the mean grain size of the polishing powder Φ. The neutron reflectivity investigations have shown that there is formation of a layer at the surface glass substrate. This layer is less dense than the bulk substrate and its thickness is around 60A. The optical and mechanical profilometry measurements have shown that both roughness and waviness decrease with P and Φ. All the experimental results show a good correlation between the neutron refractive index, the thickness and the roughness of the surface layer and the waviness of the glass surface with the two mechanical polishing parameters. The previous techniques have been completed by Secondary Ion Mass Spectroscopy and Atomic Force Microscopy measurements

Thermodynamics of poly(7-methoxy-2-acetylbenzofurane methyl methacrylate-co-styrene) and poly(2-acetylbenzofurane methyl methacrylate-co-styrene)-probe interactions at different temperatures by inverse gas chromatography

International Nuclear Information System (INIS)

İlter, Zülfiye; Demir, Abdullah; Kaya, İsmet

2016-01-01

Highlights: • Thermodynamic of methacrylate-co-styrene polymers were studied by the inverse gas chromatography. • The sorption parameters of polymer-solute systems were determined under glass transition temperature of polymers. • The solubility parameter (δ 2 ) of the polymer was obtained from the slope and intercepts. • Flory-Huggins interaction parameter (χ 12 ∞ ) were determined for polymer-solute systems. - Abstract: In this study, some thermodynamic properties of poly(7-methoxy-2-acetylbenzofurane methyl methacrylate-co-styrene) Poly(MABMM-co-St) and poly(2-acetylbenzofurane methyl methacrylate-co-styrene) Poly(ABMM-co-St) were studied by the inverse gas chromatography (IGC) technique. The retention times (t r ) of selected organic probes were determined from the interactions with Poly(MABMM-co-St) and Poly(ABMM-co-St) of four groups of solvents with different chemical natures and polarities. Then, specific volume (V g 0 ) values of probes were calculated at different column temperatures. The glass transition temperatures (T g ) of Poly(MABMM-co-St) and Poly(ABMM-co-St) were found as 393, 413 K from inverse gas chromatography measurements, respectively. Under the glass transition temperatures adsorption heat (ΔH a ) and above the glass transition molar heat (ΔH 1 S ), free energies (ΔG 1 S ) and entropies (ΔS 1 S ) belonging to sorption for every probe were calculated from inverse gas chromatography measurements. The partial molar heat (ΔH 1 ∞ ), partial molar free energy (ΔG 1 ∞ ), Flory-Huggins interaction parameter (χ 12 ∞ ) and weight fraction activity coefficient (a 1 /w 1 ) ∞ , values for infinite dilute solutions were calculated for polymer-probe systems. The solubility parameter (δ 2 ) of the polymer was obtained from the slope and intercepts of Flory-Huggins interaction parameter (χ 12 ∞ ) graphs with solubility parameters (δ 1 ) of probes.

Isolation and purification of six iridoid glycosides from gardenia jasminoides fruit by medium-pressure liquid chromatography combined with macroporous resin chromatography.

Science.gov (United States)

Wang, Yun; Liu, Hui; Shen, Lifeng; Yao, Lan; Ma, Yinlian; Yu, Dingrong; Chen, Jianhong; Li, Puling; Chen, Ying; Zhang, Cun

2015-12-01

Gardeniae fructus is one of the most frequently used herbs in traditional Chinese medicine. In the present study, a process for the enrichment of six iridoid glycosides from Gardeniae fructus was developed using medium-pressure liquid chromatography combined with macroporous resin and reversed-phase chromatography. The purities of different fractions from Gardeniae fructus were assessed using quantitative high-performance liquid chromatography. After fractionation using HPD-100 column chromatography, a 30% ethanol fraction was selected based on high-performance liquid chromatography and liquid chromatography with mass spectrometry qualitative analysis to separate and purify. Based on the orientation analysis results, six compounds-deacetyl asperulosidic acid methyl ester, gardenoside, ixoroside, scandoside methyl ester, genipin-1-O-β-d-gentiobioside, and geniposide-were successfully isolated and purified in three to four combined steps from Gardeniae fructus. The purities of these compounds were found by high-performance liquid chromatography analysis to be 97.9, 98.1, 95.5, 96.3, 97.1, and 98.7%, respectively. Moreover, their structures were elucidated by NMR spectroscopy and liquid chromatography with tandem mass spectrometry. The separation process was highly efficient, rapid, and accurate, making it a potential approach for the large-scale production of iridoids in the laboratory and providing several marker compounds for quality control. This procedure may be meaningful for the purification of other natural products used in traditional Chinese medicine. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Characterization of the efficiency of microbore liquid chromatography columns by van Deemter and kinetic plot analysis.

Science.gov (United States)

Hetzel, Terence; Loeker, Denise; Teutenberg, Thorsten; Schmidt, Torsten C

2016-10-01

The efficiency of miniaturized liquid chromatography columns with inner diameters between 200 and 300 μm has been investigated using a dedicated micro-liquid chromatography system. Fully porous, core-shell and monolithic commercially available stationary phases were compared applying van Deemter and kinetic plot analysis. The sub-2 μm fully porous as well as the 2.7 μm core-shell particle packed columns showed superior efficiency and similar values for the minimum reduced plate heights (2.56-2.69) before correction for extra-column contribution compared to normal-bore columns. Moreover, the influence of extra-column contribution was investigated to demonstrate the difference between apparent and intrinsic efficiency by replacing the column by a zero dead volume union to determine the band spreading caused by the system. It was demonstrated that 72% of the intrinsic efficiency could be reached. The results of the kinetic plot analysis indicate the superior performance of the sub-2 μm fully porous particle packed column for ultra-fast liquid chromatography. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Effect-directed analysis via hyphenated high-performance thin-layer chromatography for bioanalytical profiling of sunflower leaves.

Science.gov (United States)

Móricz, Ágnes M; Ott, Péter G; Yüce, Imanuel; Darcsi, András; Béni, Szabolcs; Morlock, Gertrud E

2018-01-19

High-performance thin-layer chromatography (HPTLC) coupled with effect-directed analysis was used for non-targeted screening of sunflower leaf extract for components exhibiting antioxidant, antibacterial and/or cholinesterase enzyme inhibitory effects. The active compounds were characterized by HPTLC-electrospray ionization-high resolution mass spectrometry (ESI-HRMS) and HPTLC-Direct Analysis in Real Time (DART)-MS/MS. The latter ambient ionization technique (less soft than ESI) resulted in oxidation and fragmentation products and characteristic fragment ions. NMR spectroscopy after targeted isolation via preparative normal phase flash chromatography and semi-preparative reversed phase high-performance liquid chromatography supported the identification of two diterpenes to be (-)-kaur-16-en-19-oic acid and 15-α-angeloyloxy-ent-kaur-16-en-19-oic acid. Both compounds found to be multi-potent as they inhibited acetylcholinesterase and butyrylcholinesterase and showed antibacterial effects against Gram-positive Bacillus subtilis and Gram-negative Aliivibrio fischeri bacteria. Kaurenoic acid was also active against the Gram-negative pepper pathogenic Xanthomonas euvesicatoria bacteria. Copyright © 2017 Elsevier B.V. All rights reserved.

ESR spectroscopy - an analytical tool for the glass industry

International Nuclear Information System (INIS)

Elvers, A.; Weissmann, R.

2001-01-01

In the past, wet chemical methods have been developed for the quantitative analysis of polyvalent elements in glasses. The major disadvantage of these chemical methods is that all structural information is lost during analysis. In addition, the analysis of species by wet chemical methods is unreliable due to possible redox reactions during the decomposition process. Therefore, the emphasis is on the physical methods which can directly detect species in bulk glasses. Especially optical and ESR spectroscopy are suitable methods due to their wide range of applications and sensitivity. Concerning quantitative measurements, no comparison between ESR results and chemical analysis of species has been published so far. This work discusses the possible application of ESR spectroscopy in the glass industry by focussing on routine interpretation, the correlation to chemical procedures and quantitative analysis. Results are presented and discussed for iron and chromium in packaging glasses. For example an excellent correlation was found between the Fe 3+ ESR signal and the chemically determined Fe 3+ concentration in glass. (orig.)

PIXE and PGAA - Complementary methods for studies on ancient glass artefacts (from Byzantine, late medieval to modern Murano glass)

Science.gov (United States)

Constantinescu, Bogdan; Cristea-Stan, Daniela; Szőkefalvi-Nagy, Zoltán; Kovács, Imre; Harsányi, Ildikó; Kasztovszky, Zsolt

2018-02-01

Combined external milli-beam Particle Induced X-ray Emission (PIXE) and Prompt Gamma Activation Analysis (PGAA) analysis was applied to characterize the composition of paste and colorants from some fragments of Byzantine bracelets (10th-12th Centuries AD), late medieval (17th-18th Centuries AD) and modern Murano glass pieces. As fluxes, PGAA revealed the samples are soda-lime glass, except four samples - two medieval vessel white shards and two dark Byzantine fragments of bracelets - which have potash flux. Aluminium was detected in various proportions in all samples indicating different sources for the added sand. The presence of Magnesium is relevant only in one bracelet fragment suggesting the use of plant (wood?) ash and confirming that the Byzantine bracelet is manufactured from the mixture of both types of glass (natron and plant ash based). PGAA also indicated the presence of low quantities of Cadmium, high level of Arsenic and Lead (possibly lead arsenate) in one medieval sample and of ZnO in Murano glass, and of CoO traces (maximum 0.1%) in all blue-colored Byzantine, late medieval to modern Murano glass artefacts. PIXE confirmed the use of small quantities of CoO for blue color, indicated Manganese combined with Iron for dark glass, Copper for green, Lead, Tin and an Arsenic compound (orpiment?) for yellow and in the case of modern Murano glass Selenium and Cadmium to obtain a reddish color. Despite PIXE - PIGE combination is probably the best one for glass analysis, our external milli-PIXE - PGAA methods proved to be adequate complementary tools to determine many chemical elements from glass composition - Si, Na, K, Ca, Al, Mg, various metallic oxides.

Analysis of Nd3+:glass, solar-pumped, high-powr laser systems

Science.gov (United States)

Zapata, L. E.; Williams, M. D.

1989-01-01

The operating characteristics of Nd(3+):glass lasers energized by a solar concentrator were analyzed for the hosts YAG, silicate glass, and phosphate glass. The modeling is based on the slab zigzag laser geometry and assumes that chemical hardening methods for glass are successful in increasing glass hardness by a factor of 4. On this basis, it was found that a realistic 1-MW solar-pumped laser might be constructed from phosphate glass 4 sq m in area and 2 mm thick. If YAG were the host medium, a 1-MW solar-pumped laser need only be 0.5 sq m in area and 0.5 cm thick, which is already possible. In addition, Nd(3+) doped glass fibers were found to be excellent solar-pumped laser candidates. The small diameter of fibers eliminates thermal stress problems, and if their diameter is kept small (10 microns), they propagate a Gaussian single mode which can be expanded and transmitted long distances in space. Fiber lasers could then be used for communications in space or could be bundled and the individual beams summed or phase-matched for high-power operation.

Corrosion of Glass Windows in DIRC PMTs

Energy Technology Data Exchange (ETDEWEB)

Va' vra, Jaroslav

2001-07-27

The DIRC photon detector contains {approx}11,000 photomultipliers (PMTs), which are submerged in ultra-pure water. This note reports on glass corrosion R and D conducted with PMTs in pure water. We conclude that only limited number ({approx}50) of the PMTs in water are affected by rapid corrosion, while a majority of the 11,000 PMTs should last, according to our measurements, for another ten years. The observation of PMT glass corrosion is based on visual observations, X-ray surface analysis, ESCA surface analysis, weight analysis, transmission measurement, as well as detailed water trace element analysis. We also correlate these observations with DIRC measurements of water pH factor, resistivity, temperature, transmission, and BaBar analysis of Bhabha and di-muon events. We also compare DIRC water purity with that of the Super Kamiokande and K2K experiments, which also use ultra-pure water. We provide empirical proof that corrosion, in our particular Borosilicate type of PMT glass window, occurs at high rate when the glass has no Zn content.

Comparison of an Electronic Nose Based on Ultrafast Gas Chromatography, Comprehensive Two-Dimensional Gas Chromatography, and Sensory Evaluation for an Analysis of Type of Whisky

Directory of Open Access Journals (Sweden)

Paulina Wiśniewska

2017-01-01

Full Text Available Whisky is one of the most popular alcoholic beverages. There are many types of whisky, for example, Scotch, Irish, and American whisky (called bourbon. The whisky market is highly diversified, and, because of this, it is important to have a method which would enable rapid quality evaluation and authentication of the type of whisky. The aim of this work was to compare 3 methods: an electronic nose based on the technology of ultrafast gas chromatography (Fast-GC, comprehensive two-dimensional gas chromatography (GC × GC, and sensory evaluation. The selected whisky brands included 6 blended whiskies from Scotland, 4 blended whiskies from Ireland, and 4 bourbons produced in the USA. For data analysis, peak heights of chromatograms were used. The panelists who took part in sensory evaluations included 4 women and 4 men. The obtained data were analyzed by 2 chemometric methods: partial least squares discriminant analysis (PLS-DA and discrimination function analysis (DFA. E-nose and GC × GC allowed for differentiation between whiskies by type. Sensory analysis did not allow for differentiation between whiskies by type, but it allowed giving consumer preferences.

Structural relaxation in annealed hyperquenched basaltic glasses

DEFF Research Database (Denmark)

Guo, Xiaoju; Mauro, John C.; Potuzak, M.

2012-01-01

The enthalpy relaxation behavior of hyperquenched (HQ) and annealed hyperquenched (AHQ) basaltic glass is investigated through calorimetric measurements. The results reveal a common onset temperature of the glass transition for all the HQ and AHQ glasses under study, indicating that the primary...... relaxation is activated at the same temperature regardless of the initial departure from equilibrium. The analysis of secondary relaxation at different annealing temperatures provides insights into the enthalpy recovery of HQ glasses....

Nuclear waste immobilization in iron phosphate glasses

International Nuclear Information System (INIS)

Garcia, D.A.; Rodriguez, Diego A.; Menghini, Jorge E.; Bevilacqua, Arturo

2007-01-01

Iron-phosphate glasses have become important in the nuclear waste immobilization area because they have some advantages over silicate-based glasses, such as a lower processing temperature and a higher nuclear waste load without losing chemical and mechanical properties. Structure and chemical properties of iron-phosphate glasses are determined in terms of the main components, in this case, phosphate oxide along with the other oxides that are added to improve some of the characteristics of the glasses. For example, Iron oxide improves chemical durability, lead oxide lowers fusion temperature and sodium oxide reduces viscosity at high temperature. In this work a study based on the composition-property relations was made. We used different techniques to characterize a series of iron-lead-phosphate glasses with uranium and aluminium oxide as simulated nuclear waste. We used the Arquimedes method to determine the bulk density, differential temperature analysis (DTA) to determine both glass transition temperature and crystallization temperature, dilatometric analysis to calculate the linear thermal expansion coefficient, chemical durability (MCC-1 test) and X-ray diffraction (XRD). We also applied some theoretic models to calculate activation energies associated with the glass transition temperature and crystallization processes. (author)

Extraction chromatography of fission products

International Nuclear Information System (INIS)

Bonnevie-Svendsen, M.; Goon, K.

1978-01-01

Various cases of using extraction chromatography during analysis of fission products are reviewed. The use of the extraction chromatography method is considered while analysing reprocessed products of nuclear fuel for quantitative radiochemical analysis and control of fission product and actinoide separation during extraction and their chemical state in production solutions. The method is used to obtain pure fractions of typical burnup monitors (neodymium, molybdenum, cerium, cesium, europium, lanthanides) during determination of nuclear fuel burnup degree. While studying the nature of nuclear reactions the method is used to separate quickly short-life isotopes, to purify β-radiator fractions before measuring their half-life periods, to enrich isotopes forming with low output during fission. Examples of using extraction chromatography are given to separate long half-life or stable fission products from spent solutions, to control environment object contamination

High-performance liquid chromatography coupled with tandem mass spectrometry technology in the analysis of Chinese Medicine Formulas: A bibliometric analysis (1997-2015).

Science.gov (United States)

He, Xi-Ran; Li, Chun-Guang; Zhu, Xiao-Shu; Li, Yuan-Qing; Jarouche, Mariam; Bensoussan, Alan; Li, Ping-Ping

2017-01-01

There is a recognized challenge in analyzing traditional Chinese medicine formulas because of their complex chemical compositions. The application of modern analytical techniques such as high-performance liquid chromatography coupled with a tandem mass spectrometry has improved the characterization of various compounds from traditional Chinese medicine formulas significantly. This study aims to conduct a bibliometric analysis to recognize the overall trend of high-performance liquid chromatography coupled with tandem mass spectrometry approaches in the analysis of traditional Chinese medicine formulas, its significance and possible underlying interactions between individual herbs in these formulas. Electronic databases were searched systematically, and the identified studies were collected and analyzed using Microsoft Access 2010, Graph Pad 5.0 software and Ucinet software package. 338 publications between 1997 and 2015 were identified, and analyzed in terms of annual growth and accumulated publications, top journals, forms of traditional Chinese medicine preparations and highly studied formulas and single herbs, as well as social network analysis of single herbs. There is a significant increase trend in using high-performance liquid chromatography coupled with tandem mass spectrometry related techniques in analysis of commonly used forms of traditional Chinese medicine formulas in the last 3 years. Stringent quality control is of great significance for the modernization and globalization of traditional Chinese medicine, and this bibliometric analysis provided the first and comprehensive summary within this field. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Analysis of Broad-band Frequency Selective Shielding Glass by FDTD method

OpenAIRE

笠嶋, 善憲; Kasashima, Yoshinori

2010-01-01

A frequency Selective shielding (FSS) glass is a print of many same size antennas on a sheet of glass, and it has high shielding properties for one specific frequency. In the past, the author analyzed theoretically the characteristics of the FSS, as a large scale array antenna. The FSS has narrow-band shielding characteristics. This time, the author analyzed accurately the characteristics of a FSS glass being a print of many same size dipole antennas on a sheet of glass by FDTD method. As the...

From the glass door to the glass ceiling: An analysis of the gender wage gap by age groups

OpenAIRE

Elena Dalla Chiara; Eleonora Matteazzi; Ilaria Petrarca

2014-01-01

Using 2009 EU-SILC data for France, Italy, the Netherlands and the United Kingdom, we decompose the gender wage gap for prime age workers. We adopt an age group approach to identify when and how the glass door and the glass ceiling effects arise and their persistency over time. The empirical results verify that the raw gender wage gap increases with age. In all considered countries, the glass ceiling effect is completely realized by the age of 30 and increases over time. French, Italian and B...

High-resolution gas chromatographic analysis of polycyclic aromatic hydrocarbons and aliphatic hydrocarbons

International Nuclear Information System (INIS)

Perez, M.; Gonzalez, D.

1988-01-01

A study of the analysis by gas chromatography of aromatic polycyclic hydrocarbons and aliphatic hydrocarbons is presented. The separation has been carried out by glass and fused silica capillary column in two different polar stationary phases OV-1 and SE-54. The limitation and the advantages of the procedure are discussed in terms of separation, sensitivity and precision. (Author) 20 refs

Analysis of sea water by difference chromatography. Final report

Energy Technology Data Exchange (ETDEWEB)

Mangelsdorf, P.C. Jr.

1977-02-01

During the final period of this research contract the principal results obtained were: (a) the development of anion analysis by difference chromatography to the extent that SO/sub 4//sup =//Cl/sup -/ can be determined to better than 0.1 percent using an 0.5 ml seawater sample, (b) the determination of the ion-exchange cation complements of a variety of sediments in river water and in seawater, and (c) the discovery of a simple technique for the qualitative removal of NH/sub 4//sup +/ from seawater samples without altering the ratios of the other cations. This method supersedes the use of Cu-Chelex which has proved impossible to sustain.

Gas chromatography in space

Science.gov (United States)

Akapo, S. O.; Dimandja, J. M.; Kojiro, D. R.; Valentin, J. R.; Carle, G. C.

1999-01-01

Gas chromatography has proven to be a very useful analytical technique for in situ analysis of extraterrestrial environments as demonstrated by its successful operation on spacecraft missions to Mars and Venus. The technique is also one of the six scientific instruments aboard the Huygens probe to explore Titan's atmosphere and surface. A review of gas chromatography in previous space missions and some recent developments in the current environment of fiscal constraints and payload size limitations are presented.

DHLW Glass Waste Package Criticality Analysis (SCPB:N/A)

International Nuclear Information System (INIS)

Davis, J.W.

1996-01-01

This analysis is prepared by the Mined Geologic Disposal System (MGDS) Waste Package Development Department (WPDD) to determine the viability of the Defense High-Level Waste (DHLW) Glass waste package concept with respect to criticality regulatory requirements in compliance with the goals of the Waste Package Implementation Plan (Ref. 5.1) for conceptual design. These design calculations are performed in sufficient detail to provide a comprehensive comparison base with other design alternatives. The objective of this evaluation is to show to what extent the concept meets the regulatory requirements or indicate additional measures that are required for the intact waste package

Gas Chromatography-Mass Spectrometric Analysis and Insecticidal ...

African Journals Online (AJOL)

Tropical Journal of Pharmaceutical Research ... apelta aerial parts was analyzed by gas chromatography/mass spectrometric (GC/MS) to determine its composition. ... into a natural fumigant/insecticide for the control of stored product insects.

Structure and properties of calcium iron phosphate glasses

Energy Technology Data Exchange (ETDEWEB)

Qian, Bin [School of Science, Southwest University of Science and Technology, Mianyang 621010 (China); Liang, Xiaofeng, E-mail: xfliangswust@gmail.com [Analytical and Testing Center, Southwest University of Science and Technology, Mianyang 621010 (China); School of Materials Science and Engineering, Southwest University of Science and Technology, Mianyang 621010 (China); Wang, Cuiling; Yang, Shiyuan [School of Materials Science and Engineering, Southwest University of Science and Technology, Mianyang 621010 (China)

2013-11-15

The structural properties of xCaO–(100 − x) (0.4Fe{sub 2}O{sub 3}–0.6P{sub 2}O{sub 5}) (x = 0, 10, 20, 30, 40, 50 mol%) glasses have been investigated by XRD, DTA, IR and Raman spectroscopy. XRD analysis has confirmed that the majority of samples are X-ray amorphous, and EDS analysis indicates that the glass matrix can accommodate ≈30 mol% CaO. IR and Raman spectra show that the glass structure consists predominantly of pyrophosphate (Q{sup 1}) units. IR spectra indicate that the phosphate network is depolymerized with the addition of CaO content. The density and glass transition temperature (T{sub g}) increase with increasing CaO content for the glasses. This behavior indicates that the addition of CaO improves the strength of the cross-links between the phosphate chains of the glass.

Analysis of Poly-β-Hydroxybutyrate in Rhizobium japonicum Bacteroids by Ion-Exclusion High-Pressure Liquid Chromatography and UV Detection †

Science.gov (United States)

Karr, Dale B.; Waters, James K.; Emerich, David W.

1983-01-01

Ion-exclusion high-pressure liquid chromatography (HPLC) was used to measure poly-β-hydroxybutyrate (PHB) in Rhizobium japonicum bacteroids. The products in the acid digest of PHB-containing material were fractionated by HPLC on Aminex HPX-87H ion-exclusion resin for organic acid analysis. Crotonic acid formed from PHB during acid digestion was detected by its intense absorbance at 210 nm. The Aminex-HPLC method provides a rapid and simple chromatographic technique for routine analysis of organic acids. Results of PHB analysis by Aminex-HPLC were confirmed by gas chromatography and spectrophotometric analysis. PMID:16346443

Nanoparticle Analysis by Online Comprehensive Two-Dimensional Liquid Chromatography combining Hydrodynamic Chromatography and Size-Exclusion Chromatography with Intermediate Sample Transformation

Science.gov (United States)

2017-01-01

Polymeric nanoparticles have become indispensable in modern society with a wide array of applications ranging from waterborne coatings to drug-carrier-delivery systems. While a large range of techniques exist to determine a multitude of properties of these particles, relating physicochemical properties of the particle to the chemical structure of the intrinsic polymers is still challenging. A novel, highly orthogonal separation system based on comprehensive two-dimensional liquid chromatography (LC × LC) has been developed. The system combines hydrodynamic chromatography (HDC) in the first-dimension to separate the particles based on their size, with ultrahigh-performance size-exclusion chromatography (SEC) in the second dimension to separate the constituting polymer molecules according to their hydrodynamic radius for each of 80 to 100 separated fractions. A chip-based mixer is incorporated to transform the sample by dissolving the separated nanoparticles from the first-dimension online in tetrahydrofuran. The polymer bands are then focused using stationary-phase-assisted modulation to enhance sensitivity, and the water from the first-dimension eluent is largely eliminated to allow interaction-free SEC. Using the developed system, the combined two-dimensional distribution of the particle-size and the molecular-size of a mixture of various polystyrene (PS) and polyacrylate (PACR) nanoparticles has been obtained within 60 min. PMID:28745485

AFM Surface Roughness and Topography Analysis of Lithium Disilicate Glass Ceramic

Directory of Open Access Journals (Sweden)

M. Pantić

2015-12-01

Full Text Available The aim of this study is presenting AFM analysis of surface roughness of Lithium disilicate glass ceramic (IPS e.max CAD under different finishing procedure (techniques: polishing, glazing and grinding. Lithium disilicate glass ceramics is all-ceramic dental system which is characterized by high aesthetic quality and it can be freely said that properties of material provide all prosthetic requirements: function, biocompatibility and aesthetic. Experimental tests of surface roughness were investigated on 4 samples with dimensions: 18 mm length, 14 mm width and 12 mm height. Contact surfaces of three samples were treated with different finishing procedure (polishing, glazing and grinding, and the contact surface of the raw material is investigated as a fourth sample. Experimental measurements were done using the Atomic Force Microscopy (AFM of NT-MDT manufacturers, in the contact mode. All obtained results of different prepared samples are presented in the form of specific roughness parameters (Rа, Rz, Rmax, Rq and 3D surface topography.

Superconducting phase of YBa2Cu3O7-δ films in high magnetic fields: Vortex glass or Bose glass

International Nuclear Information System (INIS)

Woeltgens, P.J.M.; Dekker, C.; Swueste, J.; de Wijn, H.W.

1993-01-01

Nonlinear current-voltage (I-V) curves are measured in laser-ablated YBa 2 Cu 3 O 7-δ films deposited onto SrTiO 3 . The measurements are performed near the glass phase transition in a magnetic field of 5 T at various angles from the c axis. From a critical scaling analysis, the angular dependencies of the glass transition temperature and the critical glass exponents are extracted. At small angles, these results distinguish between a vortex glass, caused by random pointlike disorder, and a Bose glass, caused by linelike disorder. The results can be understood in terms of the vortex-glass model only. No evidence is found for the existence of a Bose-glass phase

A comparative property investigation of lithium phosphate glass

Indian Academy of Sciences (India)

The present study addresses the application of microwave (MW) energy for melting lithium phosphate glass. Acomparative analysis of the properties is presented with glasses melted in conventional resistance heating adopting standardmethods of characterization. The density of the glass was found less in MW heating.

Design and Analysis of Drive Shaft using Kevlar/Epoxy and Glass/Epoxy as a Composite Material

Science.gov (United States)

Karthikeyan, P.; Gobinath, R.; Kumar, L. Ajith; Jenish, D. Xavier

2017-05-01

In automobile industry drive shaft is one of the most important components to transmit power form the engine to rear wheel through the differential gear. Generally steel drive shaft is used in automobile industry, nowadays they are more interested to replace steel drive shaft with that of composite drive shaft. The overall objective of this paper is to analyze the composite drive shaft using to find out the best replacement for conventional steel drive shaft. The uses of advanced composite materials such as Kevlar, Graphite, Carbon and Glass with proper resins ware resulted in remarkable achievements in automobile industry because of its greater specific strength and specific modulus, improved fatigue and corrosion resistances and reduction in energy requirements due to reduction in weight as compared to steel shaft. This paper is to presents, the modeling and analysis of drive shaft using Kevlar/Epoxy and Glass/Epoxy as a composite material and to find best replacement for conventional steel drive shafts with an Kevlar/epoxy or Glass/Epoxy resin composite drive shaft. Modeling is done using CATIA software and Analysis is carried out by using ANSYS 10.0 software for easy understanding. The composite drive shaft reduces the weight by 81.67 % for Kevlar/Epoxy and 72.66% for Glass/Epoxy when compared with conventional steel drive shaft.

Crafting glass vessels: current research on the ancient glass collections in the Freer Gallery of Art, Washington, D.C.

Science.gov (United States)

Nagel, Alexander; McCarthy, Blythe; Bowe, Stacy

Our knowledge of glass production in ancient Egypt has been well augmented by the publication of recently excavated materials and glass workshops, but also by more recent materials analysis, and experiments of modern glass-makers attempting to reconstruct the production process of thin-walled coreformed glass vessels. From the mounting of a prefabricated core to the final glass product our understanding of this profession has much improved. The small but well preserved glass collection of the Freer Gallery of Art in Washington, D.C. is a valid tool for examining and studying the technology and production of ancient Egyptian core formed glass vessels. Charles Lang Freer (1854-1919) acquired most of the material from Giovanni Dattari in Cairo in 1909. Previously the glass had received only limited discussion, suggesting that most of these vessels were produced in the 18th Dynasty in the 15th and 14th centuries BCE, while others date from the Hellenistic period and later. In an ongoing project we conducted computed radiography in conjunction with qualitative x-ray fluorescence analysis on a selected group of vessels to understand further aspects of the ancient production process. This paper will provide an overview of our recent research and present our data-gathering process and preliminary results. How can the examinations of core formed glass vessels in the Freer Gallery contribute to our understanding of ancient glass production and technology? By focusing on new ways of looking at old assumptions using the Freer Gallery glass collections, we hope to increase understanding of the challenges of the production process of core-vessel technology as represented by these vessels.

Gas chromatography x gas chromatography-time-of-flight mass spectrometry analysis and antibacterial activity of essential oil from Amomum xanthophlebium

International Nuclear Information System (INIS)

Masila, A.; Aminah, I.; Yaakob, W.A.; Nazlina, I.

2011-01-01

Essential oils of fresh leaves, stem, rhizomes and whole aromatic plants of Amomum xanthophlebium (Zingiberaceae) were obtained by hydro distillation. Percentage yields of the leaf, stem and whole plant oils were 0.0032, 0.0074 and 0.0021 % whereas the rhizome oil obtained was very little. Chemical components of each oil and their percentages were determined by Gas Chromatography x Gas Chromatography-Time-of-Flight Mass Spectrometry (GCxGC-TOFMS). Analysis of A. xanthophlebium oils showed that they were dominated by terpenes. Main components in the leaves were allo-aromadendrene (3.41 %), (±)-globulol (2.58 %) and rosifoliol (2.55 %); stem, α-terpineol (4.25 %), rosifoliol (2.41 %) and bingpian (2.27 %); rhizomes, viridiflorol (5.72 %), (±)-globulol (5.23 %) and α-cadinol (4.81 %); whole plants, eucalyptol (4.11 %), l-α-terpineol (2.88 %) and rosifoliol (2.82 %). The stem oil of A. xanthophlebium showed antibacterial activity against Gram-negative Escherichia coli and Gram-positive methicillin-resistant Staphylococcus aureus (MRSA) at the minimum inhibitory concentration of 80 mg/ ml. (author)

Ionic conductivities of lithium phosphorus oxynitride glasses, polycrystals, and thin films

Energy Technology Data Exchange (ETDEWEB)

Wang, B.; Bates, J.B.; Chakoumakos, B.C.; Sales, B.C.; Kwak, B.S.; Zuhr, R.A. [Oak Ridge National Lab., TN (United States); Robertson, J.D. [Univ. of Kentucky, Lexington, KY (United States). Dept. of Chemistry

1994-11-01

Various lithium phosphorus oxynitrides have been prepared in the form of glasses, polycrystals, and thin films. The structures of these compounds were investigated by X-ray and neutron diffraction, X-ray photoelectron spectroscopy (XPS), and high-performance liquid chromatography (HPLC). The ac impedance measurements indicate a significant improvement of ionic conductivity as the result of incorporation of nitrogen into the structure. In the case of polycrystalline Li{sub 2.88}PO{sub 3.73}N{sub 0.14} with the {gamma}-Li{sub 3}PO{sub 4} structure, the conductivity increased by several orders of magnitude on small addition of nitrogen. The highest conductivities in the bulk glasses and thin films were found to be 3.0 {times} 10{sup -7} and 8.9 {times} 10{sup -7} S{center_dot}cm{sup -1} at 25{degrees}C, respectively.

Characterization of glass and glass ceramic nuclear waste forms

International Nuclear Information System (INIS)

Lutze, W.; Borchardt, J.; De, A.K.

1979-01-01

Characteristics of solidified nuclear waste forms, glass and glass ceramic compositions and the properties (composition, thermal stability, crystallization, phase behavior, chemical stability, mechanical stability, and radiation effects) of glasses and glass ceramics are discussed. The preparation of glass ceramics may be an optional step for proposed vitrification plants if tailored glasses are used. Glass ceramics exhibit some improved properties with respect to glasses. The overall leach resistance is similar to that of glasses. An increased leach resistance may become effective for single radionuclides being hosted in highly insoluble crystal phases mainly when higher melting temperatures are applicable in order to get more leach resistant residual glass phases. The development of glass ceramic is going on. The technological feasibility is still to be demonstrated. The potential gain of stability when using glass ceramics qualifies the material as an alternative nuclear waste form

New insight on glass-forming ability and designing Cu-based bulk metallic glasses: The solidification range perspective

International Nuclear Information System (INIS)

Wu, Jili; Pan, Ye; Li, Xingzhou; Wang, Xianfei

2014-01-01

Highlights: • The equation, T rg = T g /T l , was rotationally modified to T rg = κ(T m /T l ) + C/T l . • The newly generalized equation suggests a way for describing glass-forming ability. • Several new Cu-based bulk metallic glasses were discovered by solidification range. - Abstract: In this paper, a new equation was rationally generalized from the reduced glass transition temperature. This equation indicates that solidification range can be used for describing glass-forming ability, which can be calculated with the aid of computational thermodynamic approach. Based on this scenario, several new Cu-based bulk metallic glasses in the ternary Cu–Zr–Ti alloy system were discovered. The as-cast samples were characterized by X-ray diffraction and transmission electronic microscopy. The results indicate that as-cast samples have monolithic amorphous nature. Thermal analysis validates that the smaller solidification range is closely related to the higher glass-forming ability, which is contributed to the effect of solidification time on the formation of bulk metallic glasses. This work also suggests that solidus can influence glass formation

Glass transition and density fluctuations in the fragile glass former orthoterphenyl

International Nuclear Information System (INIS)

Monaco, G.; Fioretto, D.; Comez, L.; Ruocco, G.

2001-01-01

High-resolution Brillouin light scattering is used to measure the dynamic structure factor of the fragile glass former orthoterphenyl (OTP) in a wide temperature range around the glass transition region and up to the boiling point. The whole set of spectra is described in terms of a phenomenological generalized hydrodynamic model. In the supercooled phase, we show the contemporary existence of the structural process, whose main features come out to be consistent with the results obtained with other spectroscopies, and of a secondary, activated process, which occurs on the 10 -11 s time scale and has a low activation energy (E a f =0.28 kcal/mol). This latter process, which is also present in the glassy phase and seems to be insensitive to the glass transition, is attributed to the coupling between the density modes and intramolecular degrees of freedom. In the normal liquid phase, the two processes merge together, and the resulting characteristic time is no longer consistent with those derived with other spectroscopies. The analysis points to the conclusion that, for what concerns the long-wavelength density fluctuations in fragile glass formers such as OTP, the universal dynamical features related to the glass transition come out clearly only in the supercooled phase and at frequencies lower than ∼10 6 Hz

Toxic Compounds Analysis With High Performance Liquid Chromatography Detected By Electro Chemical Detector (Ecd)

OpenAIRE

Hideharu Shintaniq

2014-01-01

The principal area of application of high performance liquid chromatography-electrochemical detector (HPLC-ECD) has been in the analysis of naturally-occurring analytes, such as catecholamines, and pharmaceuticals in biological samples, HPLC-ECD has also applied to the analysis of pesticides and other analytes of interest to the toxicologist. In this paper, toxic area is described. In these, ammatoxins, aromatic amine, nitro-compounds, algal toxins, fungal toxins, pesticides, veterinary drug ...

Role of SrO on the bioactivity behavior of some ternary borate glasses and their glass ceramic derivatives

Science.gov (United States)

Abdelghany, A. M.; Ouis, M. A.; Azooz, M. A.; ElBatal, H. A.; El-Bassyouni, G. T.

2016-01-01

Borate glasses containing SrO substituting both CaO and NaO were prepared and characterized for their bioactivity or bone bonding ability. Glass ceramic derivatives were prepared by thermal heat treatment process. FTIR, XRD and SEM measurements for the prepared glass and glass-ceramics before and after immersion in sodium phosphate solution for one and two weeks were carried out. The appearance of two IR peaks within the range 550-680 cm-1 after immersion in phosphate solution indicates the formation of hydroxyapatite or equivalent Sr phosphate layer. X-ray diffraction data agree with the FTIR spectral analysis. The solubility test was carried out for both glasses and glass ceramics derivatives in the same phosphate solution. The introduction of SrO increases the solubility for both glasses and glass ceramics and this is assumed to be due to the formation of Sr phosphate which is more soluble than calcium phosphate (hydroxyapatite). SEM images reveal varying changes in the surfaces of glass ceramics after immersion according to the SrO content.

Role of SrO on the bioactivity behavior of some ternary borate glasses and their glass ceramic derivatives.

Science.gov (United States)

Abdelghany, A M; Ouis, M A; Azooz, M A; ElBatal, H A; El-Bassyouni, G T

2016-01-05

Borate glasses containing SrO substituting both CaO and NaO were prepared and characterized for their bioactivity or bone bonding ability. Glass ceramic derivatives were prepared by thermal heat treatment process. FTIR, XRD and SEM measurements for the prepared glass and glass-ceramics before and after immersion in sodium phosphate solution for one and two weeks were carried out. The appearance of two IR peaks within the range 550-680cm(-1) after immersion in phosphate solution indicates the formation of hydroxyapatite or equivalent Sr phosphate layer. X-ray diffraction data agree with the FTIR spectral analysis. The solubility test was carried out for both glasses and glass ceramics derivatives in the same phosphate solution. The introduction of SrO increases the solubility for both glasses and glass ceramics and this is assumed to be due to the formation of Sr phosphate which is more soluble than calcium phosphate (hydroxyapatite). SEM images reveal varying changes in the surfaces of glass ceramics after immersion according to the SrO content. Copyright © 2015 Elsevier B.V. All rights reserved.

Analysis of the mechanical and thermal properties of jute and glass fiber as reinforcement epoxy hybrid composites

Energy Technology Data Exchange (ETDEWEB)

Braga, R.A., E-mail: roney.braga@fiat.com.br [FIAT Automóveis S.A., Teardown, CEP 32530-000 Betim, MG (Brazil); Magalhaes, P.A.A., E-mail: pamerico@pucminas.br [PUC—MINAS, Instituto Politécnico, CEP 30535-610 Belo Horizonte, MG (Brazil)

2015-11-01

This work describes the study to investigate and compare the mechanical and thermal properties of raw jute and glass fiber reinforced epoxy hybrid composites. To improve the mechanical properties, jute fiber was hybridized with glass fiber. Epoxy resin, jute and glass fibers were laminated in three weight ratios (69/31/0, 68/25/7 and 64/18/19) respectively to form composites. The tensile, flexural, impact, density, thermal and water absorption tests were carried out using hybrid composite samples. This study shows that the addition of jute fiber and glass fiber in epoxy, increases the density, the impact energy, the tensile strength and the flexural strength, but decreases the loss mass in function of temperature and the water absorption. Morphological analysis was carried out to observe fracture behavior and fiber pull-out of the samples using scanning electron microscope. - Highlights: • The work is the study of the mechanical of raw jute and glass fiber with epoxy resin. • The mechanical properties increased with more proportions of glass fibers. • The density of E69-J31-V0 was the lower. • The flexural strength did not have a significant increase. • The water absorption of E69-J31-V0 was the best.

Analysis of the mechanical and thermal properties of jute and glass fiber as reinforcement epoxy hybrid composites.

Science.gov (United States)

Braga, R A; Magalhaes, P A A

2015-11-01

This work describes the study to investigate and compare the mechanical and thermal properties of raw jute and glass fiber reinforced epoxy hybrid composites. To improve the mechanical properties, jute fiber was hybridized with glass fiber. Epoxy resin, jute and glass fibers were laminated in three weight ratios (69/31/0, 68/25/7 and 64/18/19) respectively to form composites. The tensile, flexural, impact, density, thermal and water absorption tests were carried out using hybrid composite samples. This study shows that the addition of jute fiber and glass fiber in epoxy, increases the density, the impact energy, the tensile strength and the flexural strength, but decreases the loss mass in function of temperature and the water absorption. Morphological analysis was carried out to observe fracture behavior and fiber pull-out of the samples using scanning electron microscope. Copyright © 2015 Elsevier B.V. All rights reserved.

Basaltic glasses from Iceland and the deep sea: Natural analogues to borosilicate nuclear waste-form glass

International Nuclear Information System (INIS)

Jercinovic, M.J.; Ewing, R.C.

1987-12-01

The report provides a detailed analysis of the alteration process and products for natural basaltic glasses. Information of specific applicability to the JSS project include: * The identification of typical alteration products which should be expected during the long-term corrosion process of low-silica glasses. The leached layers contain a relatively high proportion of crystalline phases, mostly in the form of smectite-type clays. Channels through the layer provide immediate access of solutions to the fresh glass/alteration layer interface. Thus, glasses are not 'protected' from further corrosion by the surface layer. * Corrosion proceeds with two rates - an initial rate in silica-undersaturated environments and a long-term rate in silica-saturated environments. This demonstrates that there is no unexpected change in corrosion rate over long periods of time. The long-term corrosion rate is consistent with that of borosilicate glasses. * Precipitation of silica-containing phases can result in increased alteration of the glass as manifested by greater alteration layer thicknesses. This emphasizes the importance of being able to predict which phases form during the reaction sequence. * For natural basaltic glasses the flow rate of water and surface area of exposed glass are critical parameters in minimizing glass alteration over long periods of time. The long-term stability of basalt glasses is enhanced when silica concentrations in solution are increased. In summary, there is considerable agreement between corrosion phenomena observed for borosilicate glasses in the laboratory and those observed for natural basalt glasses of great age. (With 121 refs.) (authors)

Development of new radiopaque glass fiber posts

Energy Technology Data Exchange (ETDEWEB)

Furtos, Gabriel, E-mail: gfurtos@yahoo.co.uk [Raluca Ripan Institute of Research in Chemistry, Babes-Bolyai University, Cluj-Napoca (Romania); Baldea, Bogdan [Dep. of Prosthodontics, Faculty of Dental Medicine, Timisoara (Romania); Silaghi-Dumitrescu, Laura [Raluca Ripan Institute of Research in Chemistry, Babes-Bolyai University, Cluj-Napoca (Romania)

2016-02-01

The aim of this study was to analyze the radiopacity and filler content of three experimental glass fiber posts (EGFP) in comparison with other glass/carbon fibers and metal posts from the dental market. Three EGFP were obtained by pultrusion of glass fibers in a polymer matrix based on 2,2-bis[4-(2-hydroxy-3-methacryloyloxypropoxy)-phenyl]propane (bis-GMA) and triethyleneglycol dimethacrylate (TEGDMA) monomers. Using intraoral sensor disks 27 posts, as well as mesiodistal sections of human molar and aluminum step wedges were radiographed for evaluation of radiopacity. The percentage compositions of fillers by weight and volume were investigated by combustion analysis. Two EGFP showed radiopacity higher than enamel. The commercial endodontic posts showed radiopacity as follows: higher than enamel, between enamel and dentin, and lower than dentin. The results showed statistically significant differences (p < 0.05) when evaluated with one-way ANOVA statistical analysis. According to combustion analyses, the filler content of the tested posts ranges between 58.84 wt.% and 86.02 wt.%. The filler content of the tested EGFP ranged between 68.91 wt.% and 79.04 wt.%. EGFP could be an alternative to commercial glass fiber posts. Future glass fiber posts are recommended to present higher radiopacity than dentin and perhaps ideally similar to or higher than that of enamel, for improved clinical detection. The posts with a lower radiopacity than dentin should be considered insufficiently radiopaque. The radiopacity of some glass fiber posts is not greatly influenced by the amount of filler. - Highlights: • AR glass fibers for dental applications • AR glass fibers have a great potential for obtaining radiopaque glass fiber posts. • Experimental AR glass fiber posts could be an alternative to commercial glass fiber posts for clinical application.

Development of new radiopaque glass fiber posts

International Nuclear Information System (INIS)

Furtos, Gabriel; Baldea, Bogdan; Silaghi-Dumitrescu, Laura

2016-01-01

The aim of this study was to analyze the radiopacity and filler content of three experimental glass fiber posts (EGFP) in comparison with other glass/carbon fibers and metal posts from the dental market. Three EGFP were obtained by pultrusion of glass fibers in a polymer matrix based on 2,2-bis[4-(2-hydroxy-3-methacryloyloxypropoxy)-phenyl]propane (bis-GMA) and triethyleneglycol dimethacrylate (TEGDMA) monomers. Using intraoral sensor disks 27 posts, as well as mesiodistal sections of human molar and aluminum step wedges were radiographed for evaluation of radiopacity. The percentage compositions of fillers by weight and volume were investigated by combustion analysis. Two EGFP showed radiopacity higher than enamel. The commercial endodontic posts showed radiopacity as follows: higher than enamel, between enamel and dentin, and lower than dentin. The results showed statistically significant differences (p < 0.05) when evaluated with one-way ANOVA statistical analysis. According to combustion analyses, the filler content of the tested posts ranges between 58.84 wt.% and 86.02 wt.%. The filler content of the tested EGFP ranged between 68.91 wt.% and 79.04 wt.%. EGFP could be an alternative to commercial glass fiber posts. Future glass fiber posts are recommended to present higher radiopacity than dentin and perhaps ideally similar to or higher than that of enamel, for improved clinical detection. The posts with a lower radiopacity than dentin should be considered insufficiently radiopaque. The radiopacity of some glass fiber posts is not greatly influenced by the amount of filler. - Highlights: • AR glass fibers for dental applications • AR glass fibers have a great potential for obtaining radiopaque glass fiber posts. • Experimental AR glass fiber posts could be an alternative to commercial glass fiber posts for clinical application.

Thermal analysis of sulfide Ge-Ga glasses doped by praseodymium

Czech Academy of Sciences Publication Activity Database

Drabik, M.; Kozak, T.; Ležal, Dimitrij; Poulain, M.; Kalužný, J.

2002-01-01

Roč. 67, č. 1 (2002), s. 223-227 ISSN 1418-2874 Institutional research plan: CEZ:AV0Z4032918 Keywords : glass transition * Pr dopand * sulfide Ge-Ga glasses Subject RIV: CA - Inorganic Chemistry Impact factor: 0.598, year: 2002

Thermal stability and Judd-Ofelt analysis of optical properties of Sm3+-doped sodium tellurite glasses

Science.gov (United States)

Mawlud, Saman Q.; Ameena, Mudhafar M.; Sahar, Md. Rahim; Mahraz, Zahra A. Said; Ahmed, Kasim Fawzy

2017-09-01

Series of glasses based on (70-x) TeO2 - 20Na2O - xSm2O3 (x=0, 0.3, 0.6, 1, 1.2, 1.5 mol%) have been prepared using melt-quenching technique. The nature of the glass has been confirmed using X-ray diffraction; it is found that the glass samples are amorphous in nature. The thermal stability of the glass has been determined by means of Differential Thermal Analysis (DTA). From the DTA curve, the glass transition temperature (Tg), crystallization temperature (Tc) and melting temperature (Tm) have been identified and thermal stability is also calculated. The absorption properties of these samples are obtained by using UV-Visible-NIR spectrometer, the recorded absorption spectra exhibit nine absorption transition bands peaks corresponding to the transitions from ground level 6H5/2→6P3/2, 4I11/2, 6F11/2, 6F9/2, 6F7/2, 6F5/2, 6F3/2, 6H15/2 and 6F1/2. The emission characteristic of this glass is characterized using Photoluminescence (PL) spectroscopy at excited wavelength 404 nm, the emission spectra consisted of four emission bands at 561.95 nm, 598.69 nm, 643.77 nm and 704.56 nm which were assigned as a transition 4G5/2→6H5/2, 6H7/2, 6H9/2 and 6H11/2 respectively. From f-f intensity model the experimental oscillator strengths, fexp and theoretical oscillator strength fcal were calculated. Using Judd-Ofelt theory and fit process of least square, the phenomenological intensity parameters Ωλ (λ=2,4,6) were obtained, In order to evaluate potential applications of Sm3+ ions in telluride glasses, the spectroscopic parameters: transition probability AR, branching ratio Br, radiative life time τr, emission pick cross section σλ for each band were calculated. The comparative studies with other Sm3+ doped different glasses showed that present glasses could be a potential candidate for lasers.

The applicability of alkaline-resistant glass fiber in cement mortar of road pavement: Corrosion mechanism and performance analysis

Directory of Open Access Journals (Sweden)

Qin Xiaochun

2017-11-01

Full Text Available The main technical requirements of road pavement concrete are high flexural strength and fatigue durability. Adding glass fiber into concrete could greatly increase flexural strength and wearing resistance of concrete. However, glass fiber has the great potential of corrosion during the cement hydration, which will directly affect the long-term performance and strength stability. In this paper, accelerated corrosion experiments have been done to find out the corrosion mechanism and property of alkali-resistant glass fiber in cement mortar. The applicability and practicability of alkaline-resistant glass fiber in road concrete have been illustrated in the analysis of flexural strength changing trend of cement mortar mixed with different proportions of activated additives to protect the corrosion of glass fiber by cement mortar. The results have shown that a 30% addition of fly ash or 10% addition of silica fume to cement matrix could effectively improve the corrosion resistance of alkali-resistant glass fiber. The optimal mixing amount of alkali-resistant glass fiber should be about 1.0 kg/m3 in consideration of ensuring the compressive strength of reinforced concrete in road pavement. The closest-packing method has been adopted in the mixture ratio design of alkali-resistant glass fiber reinforced concrete, not only to reduce the alkalinity of the cement matrix through large amount addition of activated additives but also to greatly enhance the flexural performance of concrete with the split pressure ratio improvement of 12.5–16.7%. The results suggested a prosperous application prospect for alkaline-resistant glass fiber reinforced concrete in road pavement.

Late Byzantine mineral soda high alumina glasses from Asia Minor: a new primary glass production group.

Directory of Open Access Journals (Sweden)

Nadine Schibille

Full Text Available The chemical characterisation of archaeological glass allows the discrimination between different glass groups and the identification of raw materials and technological traditions of their production. Several lines of evidence point towards the large-scale production of first millennium CE glass in a limited number of glass making factories from a mixture of Egyptian mineral soda and a locally available silica source. Fundamental changes in the manufacturing processes occurred from the eight/ninth century CE onwards, when Egyptian mineral soda was gradually replaced by soda-rich plant ash in Egypt as well as the Islamic Middle East. In order to elucidate the supply and consumption of glass during this transitional period, 31 glass samples from the assemblage found at Pergamon (Turkey that date to the fourth to fourteenth centuries CE were analysed by electron microprobe analysis (EPMA and by laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS. The statistical evaluation of the data revealed that the Byzantine glasses from Pergamon represent at least three different glass production technologies, one of which had not previously been recognised in the glass making traditions of the Mediterranean. While the chemical characteristics of the late antique and early medieval fragments confirm the current model of glass production and distribution at the time, the elemental make-up of the majority of the eighth- to fourteenth-century glasses from Pergamon indicate the existence of a late Byzantine glass type that is characterised by high alumina levels. Judging from the trace element patterns and elevated boron and lithium concentrations, these glasses were produced with a mineral soda different to the Egyptian natron from the Wadi Natrun, suggesting a possible regional Byzantine primary glass production in Asia Minor.

Direct uranium isotope ratio analysis of single micrometer-sized glass particles.

Science.gov (United States)

Kappel, Stefanie; Boulyga, Sergei F; Prohaska, Thomas

2012-11-01

We present the application of nanosecond laser ablation (LA) coupled to a 'Nu Plasma HR' multi collector inductively coupled plasma mass spectrometer (MC-ICP-MS) for the direct analysis of U isotope ratios in single, 10-20 μm-sized, U-doped glass particles. Method development included studies with respect to (1) external correction of the measured U isotope ratios in glass particles, (2) the applied laser ablation carrier gas (i.e. Ar versus He) and (3) the accurate determination of lower abundant (236)U/(238)U isotope ratios (i.e. 10(-5)). In addition, a data processing procedure was developed for evaluation of transient signals, which is of potential use for routine application of the developed method. We demonstrate that the developed method is reliable and well suited for determining U isotope ratios of individual particles. Analyses of twenty-eight S1 glass particles, measured under optimized conditions, yielded average biases of less than 0.6% from the certified values for (234)U/(238)U and (235)U/(238)U ratios. Experimental results obtained for (236)U/(238)U isotope ratios deviated by less than -2.5% from the certified values. Expanded relative total combined standard uncertainties U(c) (k = 2) of 2.6%, 1.4% and 5.8% were calculated for (234)U/(238)U, (235)U/(238)U and (236)U/(238)U, respectively. Copyright © 2012 Elsevier Ltd. All rights reserved.

Glass Transition, Crystallization of Glass-Forming Melts, and Entropy

Directory of Open Access Journals (Sweden)

Jürn W. P. Schmelzer

2018-02-01

Full Text Available A critical analysis of possible (including some newly proposed definitions of the vitreous state and the glass transition is performed and an overview of kinetic criteria of vitrification is presented. On the basis of these results, recent controversial discussions on the possible values of the residual entropy of glasses are reviewed. Our conclusion is that the treatment of vitrification as a process of continuously breaking ergodicity with entropy loss and a residual entropy tending to zero in the limit of zero absolute temperature is in disagreement with the absolute majority of experimental and theoretical investigations of this process and the nature of the vitreous state. This conclusion is illustrated by model computations. In addition to the main conclusion derived from these computations, they are employed as a test for several suggestions concerning the behavior of thermodynamic coefficients in the glass transition range. Further, a brief review is given on possible ways of resolving the Kauzmann paradox and its implications with respect to the validity of the third law of thermodynamics. It is shown that neither in its primary formulations nor in its consequences does the Kauzmann paradox result in contradictions with any basic laws of nature. Such contradictions are excluded by either crystallization (not associated with a pseudospinodal as suggested by Kauzmann or a conventional (and not an ideal glass transition. Some further so far widely unexplored directions of research on the interplay between crystallization and glass transition are anticipated, in which entropy may play—beyond the topics widely discussed and reviewed here—a major role.

Ongoing Model Development Analyzing Glass Fracture

DEFF Research Database (Denmark)

Molnar, G.; Bojtar, I.; Nielsen, Jens Henrik

2013-01-01

Present subject deals with an ongoing experimental and numerical analysis of inplane loaded glass plates. The main goal of the investigation is to develop a hybrid – discrete and finite element – model which could follow the fracture process in annealed and in tempered glass. Measurements of the ...... an overview of the structure of the research and a summary of current status archived so far.......Present subject deals with an ongoing experimental and numerical analysis of inplane loaded glass plates. The main goal of the investigation is to develop a hybrid – discrete and finite element – model which could follow the fracture process in annealed and in tempered glass. Measurements...... of the residual stress state before failure and high-speed camera recordings of the failure are being performed in order to verify the numerical model. The primary goal of this research is to follow the overall fracture of a structural element – e.g. beam – loaded inplane. Present paper would like to give...

Speciation analysis of cobalt in foods by high-performance liquid chromatography and neutron activation analysis

International Nuclear Information System (INIS)

Muto, Toshio; Koyama, Motoko

1994-01-01

A combined method by coupling high-performance liquid chromatography (HPLC, as a separation method) with neutron activation analysis (as a detection method) have been applied to the speciation analysis of cobalt in daily foods (e.g. egg, fish and milk). Cobalt species including free cobalt, vitamin B 12 and protein-bound cobalt were separated with a preparative HPLC and a centrifuge. Subsequently, the determination of cobalt in the separated species was made by neutron activation analysis. The results showed that the content of the total cobalt in the foods was found to lie in the range 0.4-11ng/g(0.4-11ppb) based on wet weight. The compositions of free cobalt, vitamin B 12 and protein-bound cobalt were ranged 16-43%, 55-73%, 2.3-17%, respectively. These experimental evidences suggest that the combination of HPLC and neutron activation analysis is expected to be a useful tool for speciation analysis of trace elements in biological as well as environmental materials. (author)

Micellar liquid chromatography

International Nuclear Information System (INIS)

Basova, Elena M; Ivanov, Vadim M; Shpigun, Oleg A

1999-01-01

Background and possibilities of practical applications of micellar liquid chromatography (MLC) are considered. Various retention models in MLC, the effects of the nature and concentration of surfactants and organic modifiers, pH, temperature and ionic strength on the MLC efficiency and selectivity are discussed. The advantages and limitations of MLC are demonstrated. The performance of MLC is critically evaluated in relationship to the reversed-phase HPLC and ion-pair chromatography. The potential of application of MLC for the analysis of pharmaceuticals including that in biological fluids and separation of inorganic anions, transition metal cations, metal chelates and heteropoly compounds is described. The bibliography includes 146 references.

Joint M3 and Diviner Analysis of the Mineralogy, Glass Composition, and Country Rock Content of Pyroclastic Deposits in Oppenheimer Crater

Science.gov (United States)

Bennett, Kristen A.; Horgan, Briony H. N.; Greenhagen, Benjamin T.; Allen, Carlton C.; Paige, David A.; Bell, James F., III

2013-01-01

Here we present our analysis of the near- and mid-infrared spectral properties of pyroclastic deposits within the floor fractured Oppenheimer Crater that are hypothesized to be Vulcanian in origin. These are the first results of our global study of lunar pyroclastic deposits aimed at constraining the range of eruption processes on the Moon. In the near-infrared, we have employed a new method of spectral analysis developed in Horgan et al. (2013) of the 1 ?m iron absorption band in Chandrayaan-1 Moon Mineralogy Mapper (M3) spectra. By analyzing both the position and shape of the 1 ?m band we can detect and map the distribution of minerals, glasses, and mixtures of these phases in pyroclastic deposits. We are also using mid-infrared spectra from the Lunar Reconnaissance Orbiter Diviner Lunar Radiometer Experiment to develop 200 m/pixel Christiansen Feature (CF) maps, which correlate with silica abundance. One of the benefits of using CF maps for analysis of pyroclastic deposits is that they can be used to detect silicic country rock that may have been emplaced by Vulcanian-style eruptions, and are sensitive to iron abundance in glasses, neither of which is possible in the near-infrared. M3 analysis reveals that the primary spectral endmembers are low-calcium pyroxene and iron-bearing glass, with only minor high-calcium pyroxene, and no detectable olivine. The large deposit in the south shows higher and more extensive glass concentrations than the surrounding deposits. We interpret the M3 spectra of the pyroclastic deposits as indicating a mixture of low-calcium pyroxene country rock and juvenile glass, and no significant olivine. Analysis of Diviner CF maps of the Oppenheimer crater floor indicates an average CF value of 8.16, consistent with a mixture of primarily plagioclase and some pyroxene. The average CF values of the pyroclastic deposits range from 8.31 in the SW to 8.24 in the SE. Since CF values within the deposits are as high as 8.49, the lower average CF

DEFENSE HIGH LEVEL WASTE GLASS DEGRADATION

International Nuclear Information System (INIS)

Ebert, W.

2001-01-01

The purpose of this Analysis/Model Report (AMR) is to document the analyses that were done to develop models for radionuclide release from high-level waste (HLW) glass dissolution that can be integrated into performance assessment (PA) calculations conducted to support site recommendation and license application for the Yucca Mountain site. This report was developed in accordance with the ''Technical Work Plan for Waste Form Degradation Process Model Report for SR'' (CRWMS M andO 2000a). It specifically addresses the item, ''Defense High Level Waste Glass Degradation'', of the product technical work plan. The AP-3.15Q Attachment 1 screening criteria determines the importance for its intended use of the HLW glass model derived herein to be in the category ''Other Factors for the Postclosure Safety Case-Waste Form Performance'', and thus indicates that this factor does not contribute significantly to the postclosure safety strategy. Because the release of radionuclides from the glass will depend on the prior dissolution of the glass, the dissolution rate of the glass imposes an upper bound on the radionuclide release rate. The approach taken to provide a bound for the radionuclide release is to develop models that can be used to calculate the dissolution rate of waste glass when contacted by water in the disposal site. The release rate of a particular radionuclide can then be calculated by multiplying the glass dissolution rate by the mass fraction of that radionuclide in the glass and by the surface area of glass contacted by water. The scope includes consideration of the three modes by which water may contact waste glass in the disposal system: contact by humid air, dripping water, and immersion. The models for glass dissolution under these contact modes are all based on the rate expression for aqueous dissolution of borosilicate glasses. The mechanism and rate expression for aqueous dissolution are adequately understood; the analyses in this AMR were conducted to

Development of conjugate methods with gas chromatography for inorganic compounds analysis

International Nuclear Information System (INIS)

Baccan, N.

1975-01-01

The application of gas chromatography combined with mass spectrometry or with nuclear methods for the analysis of inorganic compounds is studied. The advantages of the use of a gas chromatograph coupled with a quadrupole mass spectrometer or with a high resolution radiation detector, are discussed. We also studied the formation and solvent extraction of metal chelates; an aliquot of the organic phase was directly injected into the gas chromatograph and the eluted compounds were detected by mass spectrometry or, when radioactive, by nuclear methods. (author)

An Economic Theory of Glass Ceiling

OpenAIRE

Paul A. Grout; In-Uck Park; Silvia Sonderegger

2009-01-01

In the 'glass ceiling' debate there appear to be two strongly held and opposing interpretations of the evidence, one suggesting it is really the result of gender differences and the other that there is discrimination by gender. This paper provides an economic theory of the glass ceiling and one of the main insights of our analysis is that in some real sense these two interpretations are not in conflict with each other. The glass ceiling emerges as an equilibrium phenomenon when firms compete ...

New photodegradation products of chlorpyrifos and their detection on glass, soil, and leaf surfaces

International Nuclear Information System (INIS)

Walia, S.; Dureja, P.; Mukerjee, S.K.

1988-01-01

The organophosphate insecticide chlorpyrifos was irradiated under different photochemical conditions and the products characterized by gas chromatography, mass spectrometry, and NMR spectroscopy. Irradiation of chlorpyrifos in hexane yielded dechlorinated photoproducts and cleavage products. In methanol, besides these products, chlorpyrifos gave oxons. Several new photoproducts, the formation of which apparently occurs by the displacement of 5-chloro by a methoxy substituent in the pyridyl moiety. The possibility of formation of such products on glass, soil, and leaf surfaces under the influence of UV and solar simulated light have also been explored and many new products presumably formed due to simultaneous photo-dechlorination, oxidation and hydrolytic processes were detected. Photodegradation of chlorpyrifos was rapid on a soil surface but comparatively slow on glass and leaf surfaces

The analysis of aqueous mixtures using liquid chromatography-electrospray mass spectrometry

Energy Technology Data Exchange (ETDEWEB)

Johnson, Steven [Iowa State Univ., Ames, IA (United States)

1999-02-12

The focus of this dissertation is the use of chromatographic methods coupled with electrospray mass spectrometry (ES-MS) for the determination of both organic and inorganic compounds in aqueous solutions. The combination of liquid chromatography (LC) methods and ES-MS offers one of the foremost methods for determining compounds in complex aqueous solutions. In this work, LC-ES-MS methods are devised using ion exclusion chromatography, reversed phase chromatography, and ion exchange chromatography, as well as capillary electrophoresis (CE). For an aqueous sample, these LC-ES-MS and CE-ES-MS techniques require no sample preparation or analyte derivatization, which makes it possible to observe a wide variety of analytes as they exist in solution. The majority of this work focuses on the use of LC-ES-MS for the determination of unknown products and intermediates formed during electrochemical incineration (ECI), an experimental waste remediation process. This report contains a general introduction to the project and the general conclusions. Four chapters have been removed for separate processing. Titles are: Chapter 2: Determination of small carboxylic acids by ion exclusion chromatography with electrospray mass spectrometry; Chapter 3: Electrochemical incineration of benzoquinone in aqueous media using a quaternary metal oxide electrode in the absence of a soluble supporting electrolyte; Chapter 4: The determination of electrochemical incineration products of 4-chlorophenol by liquid chromatography-electrospray mass spectrometry; and Chapter 5: Determination of small carboxylic acids by capillary electrophoresis with electrospray mass spectrometry.

Optical and spectroscopic properties of Eu-doped tellurite glasses and glass ceramics

International Nuclear Information System (INIS)

Stambouli, W.; Elhouichet, H.; Gelloz, B.; Férid, M.

2013-01-01

Tellurite glasses doped with trivalent europium were prepared by the conventional melt quenching technique, in the chemical composition of (85−x) TeO 2 +5La 2 O 3 +10TiO 2 +xEu 2 O 3 by varying the concentration of the rare-earth ion in the order 0.5, 1 and 1.5 mol%. Using Judd–Ofelt analysis, we calculated intensity parameters (Ω 2 and Ω 4 ), spontaneous emission probabilities, the radiative lifetime, luminescence branching factors, the quantum yield of luminescence, and the stimulated emission cross-sections for 5 D 0 → 7 F 2 transition. The change in optical properties with the variation of Eu 3+ ion concentration have been discussed and compared with other glasses. The luminescence intensity ratio, quantum efficiency and emission cross-section values support that the TeEu1.5 tellurite glass is a suitable candidate for red laser source applications. Optical properties for Eu 3+ doped tellurite glass, heated for different temperature, were investigated. Crystalline phases for α-TeO 2 , γ-TeO 2 and TiTe 3 O 8 system were determined by the XRD method. The effect of heat treatment on luminescence properties in the tellurite glass was discussed. By using Eu 3+ as a probe, the local structure of rare-earth ion in tellurite glass, vitro-ceramic and ceramic glass has been investigated. The evaluated J–O intensity parameters have been used to calculate different radiative and laser characteristic parameters of the 5 D 0 excited level. The large magnitudes of stimulated emission cross-section (σ e ), branching ratio (β) and Gain bandwidth (σ e ×Δλ eff ) obtained for 5 D 0 → 7 F 2 (613 nm) transition for ceramic glass indicate that the present glass ceramic is promising host material for Eu 3+ doped fiber amplifiers. The measured lifetime of 5 D 0 excited state increases with increase of the heat treatment which further indicate that some Eu 3+ ions were successfully embedded in the crystal phase and prove the low phonon energy environment of Eu 3+ ions

PIXE-PIGE analysis of late roman glass fragments

Energy Technology Data Exchange (ETDEWEB)

Gomez-Tubio, B. [Departamento de Fisica Aplicada III, Escuela de Ingenieros, Universidad de Sevilla, Camino de los Descubrimientos s/n, 41092 Sevilla (Spain)]. E-mail: tubio@us.es; Ontalba Salamanca, M.A. [Departamento de Fisica, Escuela Politecnica, Universidad de Extremadura, Avda. de la Universidad s/n, 10071 Caceres (Spain); Ortega-Feliu, I. [Centro Nacional de Aceleradores, Universidad de Sevilla, Avda. Thomas A. Edison s/n, 41092 Sevilla (Spain); Respaldiza, M.A. [Centro Nacional de Aceleradores, Universidad de Sevilla, Avda. Thomas A. Edison s/n, 41092 Sevilla (Spain); Amores Carredano, F. [Departamento de Prehistoria y Arqueologia, Universidad de Sevilla, C/Dona Maria de Padilla s/n, 41010 Sevilla (Spain); Gonzalez-Acuna, D. [Departamento de Geografia, Historia y Filosofia, Universidad Pablo de Olavide, Ctra. de Utrera Km 1, 41013 Sevilla (Spain)

2006-08-15

A set of Roman glass fragments, excavated at Sevilla and dated in the 5th century A.D., has been analysed by PIXE and PIGE techniques using the external beam set-up of the 3 MV tandem Pelletron accelerator of the CNA at the University of Sevilla. Using a simple quantification method, based on the indirect charge calculation on the sample by monitoring the X-ray induced by the proton beam on the exit window, the composition of the glasses has been determined. From the obtained results, the use of soda as flux has been inferred and colouring manufacture procedures have been identified.

Analysis of atomic mobility in a Cu38Zr46Ag8Al8 bulk metallic glass

International Nuclear Information System (INIS)

Qiao, J.C.; Pelletier, J.M.

2013-01-01

Highlights: ► Atomic mobility in Cu 38 Zr 46 Ag 8 Al 8 bulk metallic glass have been investigated by DMA. ► Loss factor is directly connected to the energy lost during application of the stress. ► Structural relaxation and crystallization induces a decrease of the atomic mobility. ► The concentration of quasi-point defects links to atomic mobility in metallic glasses. - Abstract: Atomic mobility in as-cast and annealed Cu 38 Zr 46 Ag 8 Al 8 bulk metallic glass samples is analyzed by performing dynamic mechanical analysis. The loss factor is directly connected to the energy lost during application of the stress. Structural relaxation process and crystallization lead to a decrease of the atomic mobility in the bulk metallic glass. A physical model, based on the concept of quasi point defects is introduced, to describe the atomic mobility. Movements in amorphous materials are correlated. The correlation factor χ reflects the atomic mobility in bulk metallic glasses: structural relaxation and crystallization lead to a decrease of χ, implying the reduction of atomic mobility. The evolution of elastic, visco-elastic and viscoplastic components after structural relaxation and partial crystallization state during the mechanical response has been obtained. Compared with as-cast state, structural relaxation induced an increase of elastic component and a decrease of visco-elastic component in the metallic glass.

COMPARISON OF BIOACTIVITY IN VITRO OF GLASS AND GLASS CERAMIC MATERIALS DURING SOAKING IN SBF AND DMEM MEDIUM

Directory of Open Access Journals (Sweden)

GABRIELA LUTIŠANOVÁ

2011-09-01

Full Text Available This paper investigated the surface reactivity of two sets of glasses and glass ceramic materials belonging to the Li2O–SiO2–CaO–P2O5–CaF2 system. The in vitro bioactivity of coatings was evaluated using simulated body fluid (SBF and Dulbecco’s Modified Eagle’s Medium (DMEM soaking test in static regime for up to 28 days at 36.5°C in microincubator. The surface structure changes were examined by scanning electron microscopy (SEM and electron probe micro-analyzer (EPMA methods. The functional groups of the silicate and phosphates were identified by infrared spectroscopy (IR. The crystal phases of the glasses and glass ceramics were identified by X-ray diffraction analysis (XRD. The results suggest the bioactivity behavior for all compositions of glasses as well as glass ceramic samples after 28 days in the SBF and DMEM medium. The surface characterization and in vitro tests revealed a few variations in the reactivity of the different glasses and glass ceramic samples in their pristine form. The best results show the samples of glass and glass ceramic samples with higher content of fluorapatite (FA. The use of the acellular culture medium DMEM resulted in a delay at the start of precipitation.

Phytochemical analysis of ethanolic extract of Dichrostachys Cinerea W and Arn leaves by a thin layer chromatography, high performance thin layer chromatography and column chromatography

OpenAIRE

M Vijayalakshmi; K Periyanayagam; K Kavitha; K Akilandeshwari

2013-01-01

Background: The leaves of Dichrostachys cinerea are used as laxative, diuretic, painkiller. It is also used in the treatment of gonorrhoea, boils, oedema, gout, veneral diseases and nasopharyngeal affections, etc. Materials and Methods: The Phytochemical investigation of ethanolic extract of D. cinerea leaves were performed by standard chemical tests, thin layer chromatography (TLC) by using various solvent systems, and by high performance liquid chromatography (HPTLC). Two compounds were...

Production and remediation of low sludge simulated Purex waste glasses, 2: Effects of sludge oxide additions on glass durability

International Nuclear Information System (INIS)

Ramsey, W.G.

1993-01-01

Glass produced during the Purex 4 campaigns of the Integrated DWPF Melter System (IDMS) and the 774 Research Melter contained a lower fraction of sludge components than targeted by the Product Composition Control System (PCCS). Purex 4 glass was more durable than the benchmark (EA) glass, but was less durable than most other simulated SRS high-level waste glasses. Further, the measured durability of Purex 4 glass was not as well correlated with the durability predicted from the DWPF process control algorithm, probably because the algorithm was developed to predict the durability of SRS high-level waste glasses with higher sludge content than Purex 4. A melter run, designated Purex 4 Remediation, was performed using the 774 Research Melter to determine if the initial PCCS target composition determined for Purex 4 would produce acceptable glass whose durability could be accurately modeled by the DWPF glass durability algorithm. Reagent grade oxides and carbonates were added to Purex 4 melter feed stock to simulate a higher sludge loading. Each canister of glass produced was sampled and the glass durability was determined by the Product Consistency Test method. This document details the durability data and subsequent analysis

LSA glass-ceramic tiles made by powder pressing

International Nuclear Information System (INIS)

Figueira, F.C.; Bertan, F.M.; Riella, H.G.; Uggioni, E.; Bernardin, A.M.

2009-01-01

A low cost alternative for the production of glass-ceramic materials is the pressing of the matrix glass powders and its consolidation simultaneously with crystallization in a single stage of sintering. The main objective of this work was to obtain LSA glass ceramics with low thermal expansion, processed by pressing and sintering a ceramic frit powder. The raw materials were homogenized and melted (1480 deg C, 80min), and the melt was poured in water. The glass was chemically (XRF and AAS) and thermally (DTA, 10 deg C/min, air) characterized, and then ground (60min and 120min). The ground powders were characterized (laser diffraction) and compressed (35MPa and 45MPa), thus forming four systems. The compacts were dried (150 deg C, 24h) and sintered (1175 deg C and 1185 deg C, 10 deg C/min). Finally, the glass-ceramics were characterized by microstructural analysis (SEM and XRD), mechanical behavior (σbending) and thermal analysis (α). The best results for thermal expansion were those for the glass-ceramics processed with smaller particle size and greater compaction pressure. (author)

Gas chromatography at the Tritium Laboratory Karlsruhe

International Nuclear Information System (INIS)

Laesser, R.; Gruenhagen, S.

2003-08-01

Among the analytical techniques (mass spectrometry, laser Raman spectroscopy, gas chromatography, use of ionisation chambers) employed at the Tritium Laboratory Karlsruhe (TLK), gas chromatography plays a prominent role. The main reasons for that are the simplicity of the gas chromatographic separation process, the small space required for the equipment, the low investment costs in comparison to other methods, the robustness of the equipment, the simple and straightforward analysis and the fact that all gas species of interest (with the exception of water) can easily be detected by gas chromatographic means. The conventional gas chromatographs GC1 and GC2 used in the Tritium Measurement Techniques (TMT) System of the TLK and the gas chromatograph GC3 of the experiment CAPER are presented in detail, by discussing their flow diagrams, their major components, the chromatograms measured by means of various detectors, shortcomings and possible improvements. One of the main disadvantages of the conventional gas chromatography is the long retention times required for the analysis of hydrogen gas mixtures. To overcome this disadvantage, micro gas chromatography for hydrogen analysis was developed. Reduction of the retention times by one order of magnitude was achieved. (orig.)

Study of Separation and Identification of the Active Ingredients in Gardenia jasminoides Ellis Based on a Two-Dimensional Liquid Chromatography by Coupling Reversed Phase Liquid Chromatography and Hydrophilic Interaction Liquid Chromatography.

Science.gov (United States)

Zhou, Xuan; Chen, Cen; Ye, Xiaolan; Song, Fenyun; Fan, Guorong; Wu, Fuhai

2017-01-01

In this paper, by coupling reversed phase liquid chromatography (RPLC) and hydrophilic interaction liquid chromatography (HILIC), a two-dimensional liquid chromatography system was developed for separation and identification of the active ingredients in Gardenia jasminoides Ellis (GJE). By applying the semi-preparative C18 column as the first dimension and the core-shell column as the second dimension, a total of 896 peaks of GJE were separated. Among the 896 peaks, 16 active ingredients including geniposide, gardenoside, gardoside, etc. were identified by mass spectrometry analysis. The results indicated that the proposed two-dimensional RPLC/HILIC system was an effective method for the analysis of GJE and might hold a high potential to become a useful tool for analysis of other complex mixtures. © The Author 2016. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

Electrochromic Glasses.

Science.gov (United States)

1980-07-31

this glass and that dipole-dipole correlations contribute to the "ferroelectric-like" character of this amorphous system. The TeO2 -W03 glasses can only...shows the dielectric constant and Fig. I(b) glass from pure TeO2 ot pure WO. In addition, glass the tan 8 of the WO glass as a function of temperature... glasses containing WO, in various glass forming nitworks of LifO-B1O0, Na:O-BzO,, and TeO2 were prepared from reagent grade oxides at 800 C - 9SO C in

Physical and chemical analysis of glass beads and glassy slag from Iron Age sites in northeast Thailand : preliminary findings

International Nuclear Information System (INIS)

Saitowitz, S.J.; Reid, D.L.

2001-01-01

Substantial numbers of glass beads have been found at the Iron Age site of Noen U-Loke (ca. 850 BC to AD 500) in northeast Thailand. Typological classification of the beads, using standardised procedures, together with specialized analytical data show that while distinctly different bead-making techniques were used to produce the beads, the chemical composition of the glass was very similar. This information suggests the possibility of multiple craftsmen, at varied levels of expertise, using glass made at a single source or using raw materials found within a specific region. These findings allow for more detailed physical and chemical analysis of the beads, so as to quantify the spatial and temporal variability of different bead types. A fragment of glassy slag, excavated at Noen U-Loke, was analysed to distinguish whether it could be associated with a glass making process. However, the results were unable to confirm whether it was used to make glass suitable for beads. (author). 30 refs., 12 figs., 2 tabs

Surface analysis of glass fibres using XPS and AFM: case study of glass fibres recovered from the glass fibre reinforced polymer using chemical recycling

Science.gov (United States)

Nzioka, A. M.; Kim, Y. J.

2018-01-01

In this study, we present the results of an experimental study of the use of the X-ray photoelectron spectroscopy (XPS) and atomic force microscopy (AFM) to characterise the coatings of the recovered E - glass fibres. The recovered E - glass fibres were obtained using chemical recycling process coupled with ultrasound cavitation. The objective of this study was to analyse the impact of chemical recycling and the ultrasound cavitation process on the sizing properties of the recovered fibres. We obtained the recovered fibres and sized using 1 wt% 3 - aminopropyltriethoxysilane (APS). Part of the sized fibres was washed with acetone and analysed all the sample fibres using AFM and XPS. Results showed the different composition of sizing after extraction using acetone. We compared the results of this study with that of virgin clean glass fibres.

Two-step ion-exchange chromatographic purification combined with reversed-phase chromatography to isolate C-peptide for mass spectrometric analysis.

Science.gov (United States)

Kabytaev, Kuanysh; Durairaj, Anita; Shin, Dmitriy; Rohlfing, Curt L; Connolly, Shawn; Little, Randie R; Stoyanov, Alexander V

2016-02-01

A liquid chromatography with mass spectrometry on-line platform that includes the orthogonal techniques of ion exchange and reversed phase chromatography is applied for C-peptide analysis. Additional improvement is achieved by the subsequent application of cation- and anion-exchange purification steps that allow for isolating components that have their isoelectric points in a narrow pH range before final reversed-phase mass spectrometry analysis. The utility of this approach for isolating fractions in the desired "pI window" for profiling complex mixtures is discussed. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Pseudo-absolute quantitative analysis using gas chromatography – Vacuum ultraviolet spectroscopy – A tutorial

Energy Technology Data Exchange (ETDEWEB)

Bai, Ling [Department of Chemistry & Biochemistry, The University of Texas at Arlington, Arlington, TX (United States); Smuts, Jonathan; Walsh, Phillip [VUV Analytics, Inc., Cedar Park, TX (United States); Qiu, Changling [Department of Chemistry & Biochemistry, The University of Texas at Arlington, Arlington, TX (United States); McNair, Harold M. [Department of Chemistry, Virginia Tech, Blacksburg, VA (United States); Schug, Kevin A., E-mail: kschug@uta.edu [Department of Chemistry & Biochemistry, The University of Texas at Arlington, Arlington, TX (United States)

2017-02-08

The vacuum ultraviolet detector (VUV) is a new non-destructive mass sensitive detector for gas chromatography that continuously and rapidly collects full wavelength range absorption between 120 and 240 nm. In addition to conventional methods of quantification (internal and external standard), gas chromatography - vacuum ultraviolet spectroscopy has the potential for pseudo-absolute quantification of analytes based on pre-recorded cross sections (well-defined absorptivity across the 120–240 nm wavelength range recorded by the detector) without the need for traditional calibration. The pseudo-absolute method was used in this research to experimentally evaluate the sources of sample loss and gain associated with sample introduction into a typical gas chromatograph. Standard samples of benzene and natural gas were used to assess precision and accuracy for the analysis of liquid and gaseous samples, respectively, based on the amount of analyte loaded on-column. Results indicate that injection volume, split ratio, and sampling times for splitless analysis can all contribute to inaccurate, yet precise sample introduction. For instance, an autosampler can very reproducibly inject a designated volume, but there are significant systematic errors (here, a consistently larger volume than that designated) in the actual volume introduced. The pseudo-absolute quantification capability of the vacuum ultraviolet detector provides a new means for carrying out system performance checks and potentially for solving challenging quantitative analytical problems. For practical purposes, an internal standardized approach to normalize systematic errors can be used to perform quantitative analysis with the pseudo-absolute method. - Highlights: • Gas chromatography diagnostics and quantification using VUV detector. • Absorption cross-sections for molecules enable pseudo-absolute quantitation. • Injection diagnostics reveal systematic errors in hardware settings. • Internal

Pseudo-absolute quantitative analysis using gas chromatography – Vacuum ultraviolet spectroscopy – A tutorial

International Nuclear Information System (INIS)

Bai, Ling; Smuts, Jonathan; Walsh, Phillip; Qiu, Changling; McNair, Harold M.; Schug, Kevin A.

2017-01-01

The vacuum ultraviolet detector (VUV) is a new non-destructive mass sensitive detector for gas chromatography that continuously and rapidly collects full wavelength range absorption between 120 and 240 nm. In addition to conventional methods of quantification (internal and external standard), gas chromatography - vacuum ultraviolet spectroscopy has the potential for pseudo-absolute quantification of analytes based on pre-recorded cross sections (well-defined absorptivity across the 120–240 nm wavelength range recorded by the detector) without the need for traditional calibration. The pseudo-absolute method was used in this research to experimentally evaluate the sources of sample loss and gain associated with sample introduction into a typical gas chromatograph. Standard samples of benzene and natural gas were used to assess precision and accuracy for the analysis of liquid and gaseous samples, respectively, based on the amount of analyte loaded on-column. Results indicate that injection volume, split ratio, and sampling times for splitless analysis can all contribute to inaccurate, yet precise sample introduction. For instance, an autosampler can very reproducibly inject a designated volume, but there are significant systematic errors (here, a consistently larger volume than that designated) in the actual volume introduced. The pseudo-absolute quantification capability of the vacuum ultraviolet detector provides a new means for carrying out system performance checks and potentially for solving challenging quantitative analytical problems. For practical purposes, an internal standardized approach to normalize systematic errors can be used to perform quantitative analysis with the pseudo-absolute method. - Highlights: • Gas chromatography diagnostics and quantification using VUV detector. • Absorption cross-sections for molecules enable pseudo-absolute quantitation. • Injection diagnostics reveal systematic errors in hardware settings. • Internal

Thermal analysis of chalcogenide glasses of the system (As/sub/2Se/sub/3)/sub/(1-x):(Tl/sub/2Se)/sub/x

International Nuclear Information System (INIS)

Majid, C.A.

1987-01-01

In this paper differential thermal analysis (DTA) measurements of chalcogenide glasses of the system (As/sub/2Se/sub/3)/sub/(1-x): (Tl/sub/2Se)/sub/x, with x=0, 0.125, 0.25 and 0.50 are reported. The glass-forming tendencies of these materials have been calculated. The glass-forming tendency of As/sub/2Se/sub/3 has been found to be the highest among the member glasses of this family of chalcogenides. It was found that the glass-forming tendency of As/sub/2Se/sub/3 decreasing gradually at the Tl/sub/2/Se concentration increases. Tl/sub/2Se additions lower the glass transition temperature T/sub/q and the area under the endothermic peak for glass transition temperature, suggesting a tendency for relatively weaker bonding and hence less stability of Tl-rich glass compositions. These studies show that Tl/sub/2Se concentrations result in glasses with progressively higher crystallization tendencies. (author)

REDOX state analysis of platinoid elements in simulated high-level radioactive waste glass by synchrotron radiation based EXAFS

Energy Technology Data Exchange (ETDEWEB)

Okamoto, Yoshihiro, E-mail: okamoto.yoshihiro@jaea.go.jp [Condensed Matter Chemistry Group, Quantum Beam Science Center, Japan Atomic Energy Agency, Shirakata 2-4, Tokai-mura, Ibaraki 319-1195 (Japan); Shiwaku, Hideaki [Quantum Beam Science Center, Japan Atomic Energy Agency, Kouto 1-1-1, Sayo-cho, Hyogo 679-5143 (Japan); Nakada, Masami [Nuclear Engineering Science Center, Japan Atomic Energy Agency, Shirakata 2-4, Tokai-mura, Ibaraki 319-1195 (Japan); Komamine, Satoshi; Ochi, Eiji [Japan Nuclear Fuel Limited, 4-108 Aza Okitsuke, Oaza Obuchi, Rokkasho-mura, Aomori 030-3212 (Japan); Akabori, Mitsuo [Nuclear Engineering Science Center, Japan Atomic Energy Agency, Shirakata 2-4, Tokai-mura, Ibaraki 319-1195 (Japan)

2016-04-01

Extended X-ray Absorption Fine Structure (EXAFS) analyses were performed to evaluate REDOX (REDuction and OXidation) state of platinoid elements in simulated high-level nuclear waste glass samples prepared under different conditions of temperature and atmosphere. At first, EXAFS functions were compared with those of standard materials such as RuO{sub 2}. Then structural parameters were obtained from a curve fitting analysis. In addition, a fitting analysis used a linear combination of the two standard EXAFS functions of a given elements metal and oxide was applied to determine ratio of metal/oxide in the simulated glass. The redox state of Ru was successfully evaluated from the linear combination fitting results of EXAFS functions. The ratio of metal increased at more reducing atmosphere and at higher temperatures. Chemical form of rhodium oxide in the simulated glass samples was RhO{sub 2} unlike expected Rh{sub 2}O{sub 3}. It can be estimated rhodium behaves according with ruthenium when the chemical form is oxide.

ToF-SIMS analysis for leaching studies of potash–lime–silica glass

International Nuclear Information System (INIS)

De Bardi, Monica; Hutter, Herbert; Schreiner, Manfred

2013-01-01

In this work the durability to acidic solutions of two kinds of potash–lime–silica glasses with compositions typical for mediaeval stained glass was investigated. The low amount of network formers such as silica and alumina, and the high amount of network modifiers such as potassium and calcium, give to the glass a lower chemical stability compared to modern glass. Studies on its durability are of interest to understand degradation mechanisms. In particular the leaching procedure was focused on determining any correlation between the type of acid and the corrosion of glass independently from the pH value, which was kept constant during the different acidic treatments. Time-of-flight secondary ion mass spectrometry (ToF-SIMS) is a valuable tool to study compositional variations of glass, giving useful information concerning provenance, effects of the conservation environment, of weathering or leaching processes and about the compositional differences between the corroded layer and the bulk as a function of depth. In spite of that the insulating properties of glass, the surface roughness and the parameters used for the measurements can lead to possible misinterpretations of the results; in this paper these difficulties are discussed, in order to better interpret the analyses performed on leached glass. ToF-SIMS data are influenced by strong matrix effects making quantification difficult; for this reason the quantitative composition and surface morphology of the leached layer were additionally investigated with scanning electron microscopy equipped with energy dispersive X-ray spectroscopy (SEM–EDX)

Gas chromatography/sniffing port analysis evaluated for aroma release from rehydrated French beans (Phaseolus vulgaris).

NARCIS (Netherlands)

Ruth, van S.M.; Roozen, J.P.; Cozijnsen, J.L.

1996-01-01

The technique of gas chromatography/sniffing port analysis was evaluated for studying the release of aroma compounds from rehydrated diced French beans. The aroma compounds 2-—methylbutanal and hexanal were released at a constant rate over time. An identical selection of odour active compounds was

Flow analysis from PIV in engraved champagne tasting glasses: flute versus coupe

Science.gov (United States)

Beaumont, Fabien; Liger-Belair, Gérard; Polidori, Guillaume

2015-08-01

Glass shape, and especially its open aperture, is suspected to play an important role as concerns the kinetics of CO2 and flavor release during champagne tasting. In recent years, much interest has been devoted to depict each and every parameter involved in the release of gaseous CO2 from glasses poured with champagne. One cannot understand the bubbling and aromatic exhalation events in champagne tasting, however, without studying the flow-mixing mechanisms inside the glass. Indeed, a key assumption is that a causal link may exist between flow structures created in the wine due to bubble motion and the process of CO2 release and flavor exhalation. In the present work, two quite emblematic types of champagne drinking vessels are studied. The particle image velocimetry technique has been used in order to reveal the velocity field of the liquid due to the ascending bubble-driven flow for both glasses poured with champagne. The contribution of glass shape on the flow patterns and CO2 release in both glasses are discussed by the use of experimental results. The results show that the continuous flow of ascending bubbles strongly modifies the mixing and convection conditions of the surrounding liquid medium whose behavior is strongly glass shape dependent.

The studies of post-medieval glass by multivariate and X-ray fluorescence analysis

International Nuclear Information System (INIS)

Kierzek, J.; Kunicki-Goldfinger, J.

2002-01-01

Multivariate statistical analysis of the results obtained by energy dispersive X-ray fluorescence analysis has been used in the study of baroque vessel glasses originated from central Europe. X-ray spectrometry can be applied as a completely non-destructive, non-sampling and multi-element method. It is very useful in the studies of valuable historical artefacts. For the last years, multivariate statistical analysis has been developed as an important tool for the archaeometric purposes. Cluster, principal component and discriminant analysis were applied for the classification of the examined objects. The obtained results show that these statistical tools are very useful and complementary in the studies of historical objects. (author)

The "wonderful properties of glass": Liebig's Kaliapparat and the practice of chemistry in glass.

Science.gov (United States)

Jackson, Catherine M

2015-03-01

Everybody knows that glass is and always has been an important presence in chemical laboratories. Yet the very self-evidence of this notion tends to obscure a supremely important change in chemical practice during the early decades of the nineteenth century. This essay uses manuals of specifically chemical glassblowing published between about 1825 and 1835 to show that early nineteenth-century chemists began using glass in distinctly new ways and that their appropriation of glassblowing skill had profoundly important effects on the emerging discipline of chemistry. The new practice of chemistry in glass-exemplified in this essay by Justus Liebig's introduction of a new item of chemical glassware for organic analysis, the Kaliapparat--transformed not merely the material culture of chemistry but also its geography, its pedagogy, and, ultimately, its institutions. Moving chemistry into glass--a change so important that it warrants the term "glassware revolution"--had far-reaching consequences.

Taste characteristics of Chinese bayberry juice characterized by sensory evaluation, chromatography analysis, and an electronic tongue.

Science.gov (United States)

Yu, Haiyan; Zhang, Yan; Zhao, Jie; Tian, Huaixiang

2018-05-01

To evaluate the taste characteristics of Chinese bayberry juice, four types of bayberry juice sourced from different origins and varieties were analysed using sensory evaluation, chromatography, spectroscopy analysis and an electronic tongue (E-tongue). Nine organic acids and three sugars were assessed using high performance liquid chromatography. Total polyphenols were measured by spectrophotometry. The overall taste profile was collected using the E-tongue. The four types of bayberry juice differed in the sensory attributes of sour, sweet, bitter, and astringent. The E-tongue responses combined with discriminant analysis were able to characterise the taste profiles of the juices. The relationships between the taste compounds and the sensory panel scores established by partial least squares showed that total polyphenols, quininic acid, maleic acid, fructose, citric acid, lactic acid, succinic acid and sucrose made significant contributions to the taste characteristics of the Chinese bayberry juice.

Neutral monosaccharide composition analysis of plant-derived oligo- and polysaccharides by high performance liquid chromatography.

Science.gov (United States)

Yan, Jun; Shi, Songshan; Wang, Hongwei; Liu, Ruimin; Li, Ning; Chen, Yonglin; Wang, Shunchun

2016-01-20

A novel analytical method for neutral monosaccharide composition analysis of plant-derived oligo- and polysaccharides was developed using hydrophilic interaction liquid chromatography coupled to a charged aerosol detector. The effects of column type, additives, pH and column temperature on retention and separation were evaluated. Additionally, the method could distinguish potential impurities in samples, including chloride, sulfate and sodium, from sugars. The results of validation demonstrated that this method had good linearity (R(2) ≥ 0.9981), high precision (relative standard deviation ≤ 4.43%), and adequate accuracy (94.02-103.37% recovery) and sensitivity (detection limit: 15-40 ng). Finally, the monosaccharide compositions of the polysaccharide from Eclipta prostrasta L. and stachyose were successfully profiled through this method. This report represents the first time that all of these common monosaccharides could be well-separated and determined simultaneously by high performance liquid chromatography without additional derivatization. This newly developed method is convenient, efficient and reliable for monosaccharide analysis. Copyright © 2015 Elsevier Ltd. All rights reserved.

Relaxations in spin glasses: Similarities and differences from ordinary glasses

International Nuclear Information System (INIS)

Ngai, K.L.; Rajagopal, A.K.; Huang, C.Y.

1984-01-01

Relaxation phenomena have become a major concern in the physics of spin glasses. There are certain resemblances of these relaxation properties to those of ordinary glasses. In this work, we compare the relaxation properties of spin glasses near the freezing temperature with those of glasses near the glass transition temperature. There are similarities between the two types of glasses. Moreover, the relaxation properties of many glasses and spin glasses are in conformity with two coupled ''universality'' relations predicted by a recent model of relaxations in condensed matter

Analysis of antiepileptic drugs in biological fluids by means of electrokinetic chromatography.

Science.gov (United States)

Pucci, Vincenzo; Raggi, Maria Augusta

2005-02-01

An overview of the electrokinetic chromatographic methods for the analysis of antiepileptic drug levels in biological samples is presented. In particular, micellar electrokinetic capillary chromatography is a very suitable method for the determination of these drugs, because it allows a rapid, selective, and accurate analysis. In addition to the electrokinetic chromatographic studies on the determination of antiepileptic drugs, some information regarding sample pretreatment will also be reported: this is a critical step when the analysis of biological fluids is concerned. The electrokinetic chromatographic methods for the determination of recent antiepileptic drugs (e.g., lamotrigine, levetiracetam) and classical anticonvulsants (e.g., carbamazepine, phenytoin, ethosuximide, valproic acid) will be discussed in depth, and their pharmacological profiles will be briefly described as well.

Development of a sensitive and rapid method for rifampicin impurity analysis using supercritical fluid chromatography.

Science.gov (United States)

Li, Wei; Wang, Jun; Yan, Zheng-Yu

2015-10-10

A novel simple, fast and efficient supercritical fluid chromatography (SFC) method was developed and compared with RPLC method for the separation and determination of impurities in rifampicin. The separation was performed using a packed diol column and a mobile phase B (modifier) consisting of methanol with 0.1% ammonium formate (w/v) and 2% water (v/v). Overall satisfactory resolutions and peak shapes for rifampicin quinone (RQ), rifampicin (RF), rifamycin SV (RSV), rifampicin N-oxide (RNO) and 3-formylrifamycinSV (3-FR) were obtained by optimization of the chromatography system. With gradient elution of mobile phase, all of the impurities and the active were separated within 4 min. Taking full advantage of features of SFC (such as particular selectivity, non-sloping baseline in gradient elution, and without injection solvent effects), the method was successfully used for determination of impurities in rifampicin, with more impurity peaks detected, better resolution achieved and much less analysis time needed compared with conventional reversed-phase liquid chromatography (RPLC) methods. Copyright © 2015 Elsevier B.V. All rights reserved.

The Use of Gas Chromatography for Biogas Analysis

Science.gov (United States)

Andersen, Amanda; Seeley, John; Aurandt, Jennifer

2010-04-01

Energy from natural gas accounts for 24 percent of energy consumed in the US. Natural gas is a robust form of energy which is rich in methane content and is low in impurities. This quality suggests that it is a very clean and safe gas; it can be used in providing heat, a source for cooking, and in powering vehicles. The downside is that it is a non-renewable resource. On the contrary, methane rich gas that is produced by the breakdown of organic material in an anaerobic environment, called biogas, is a renewable energy source. This research focuses on the gas analysis portion of the creation of the anaerobic digestion and verification laboratory where content and forensic analysis of biogas is performed. Gas Chromatography is implemented as the optimal analytical tool for quantifying the components of the biogas including methane, carbon dioxide, hydrogen sulfide and siloxanes. In addition, the problems associated with the undesirable components are discussed. Anaerobic digestion of primary sludge has consistently produced about 55 percent methane; future goals of this research include studying different substrates to increase the methane yield and decrease levels of impurities in the gas.

Monitoring of Miit glass solution interactions by brine analysis

International Nuclear Information System (INIS)

Sassoon, R.E.; Gong, M.; Adel-Hadadi, M.; Brandys, M.; Barkatt, A.; Macedo, P.B.

1989-01-01

Analyses of brine samples taken from borehole MIIT=8 at the WIPP site were carried out in order to study the leaching behavior of the brine in this system. The standard addition method was used with the analytical techniques of AA, DCP and ICP-MS to determine the concentration of the components in the brine. The changes in the concentration of the major components, Na, Mg and K can be explained by reactions of the brine with the rock salt walls of the borehole. From the data obtained for the other components no leaching of the SRL-Y glass discs in the test could be observed. It was however possible to determine an upper limit for leaching of the glass from isotope ratio studies made on Li which yielded a value for the leach rate of lithium from the glass of 0.117 g m -2 d -1

Replica analysis of partition-function zeros in spin-glass models

International Nuclear Information System (INIS)

Takahashi, Kazutaka

2011-01-01

We study the partition-function zeros in mean-field spin-glass models. We show that the replica method is useful to find the locations of zeros in a complex parameter plane. For the random energy model, we obtain the phase diagram in the plane and find that there are two types of distributions of zeros: two-dimensional distribution within a phase and one-dimensional one on a phase boundary. Phases with a two-dimensional distribution are characterized by a novel order parameter defined in the present replica analysis. We also discuss possible patterns of distributions by studying several systems.

Core-Shell Columns in High-Performance Liquid Chromatography: Food Analysis Applications

Science.gov (United States)

Preti, Raffaella

2016-01-01

The increased separation efficiency provided by the new technology of column packed with core-shell particles in high-performance liquid chromatography (HPLC) has resulted in their widespread diffusion in several analytical fields: from pharmaceutical, biological, environmental, and toxicological. The present paper presents their most recent applications in food analysis. Their use has proved to be particularly advantageous for the determination of compounds at trace levels or when a large amount of samples must be analyzed fast using reliable and solvent-saving apparatus. The literature hereby described shows how the outstanding performances provided by core-shell particles column on a traditional HPLC instruments are comparable to those obtained with a costly UHPLC instrumentation, making this novel column a promising key tool in food analysis. PMID:27143972

Wetting and surface tension of bismate glass melt

International Nuclear Information System (INIS)

Shim, Seung-Bo; Kim, Dong-Sun; Hwang, Seongjin; Kim, Hyungsun

2009-01-01

Lead oxide glass frits are used widely in the electronics industry for low-temperature firing. On the other hand, one of the low-sintering and low-melting lead-free glass systems available, the bismate glass system, is considered to be an alternative to lead oxide glass. In order to extend the applications of Bi 2 O 3 glasses, this study examined the thermophysical properties of low-melting Bi 2 O 3 -B 2 O 3 -ZnO-BaO-Al 2 O 3 -SiO 2 glass frits with various ZnO/B 2 O 3 ratios. The fundamental thermal properties, such as glass transition temperature and softening point, were examined by differential thermal analysis and a glass softening point determination system. The wetting angles, viscosities and surface tension of the various bismate glasses on an alumina substrate were measured using hot-stage microscopy and the sessile drop method. These thermophysical properties will be helpful in understanding the work of adhesion and the liquid spread kinetics of glass frits.

Determination of the origin of the medieval glass bracelets discovered in Dubna, Moscow Region, Russia, using the neutron activation analysis

International Nuclear Information System (INIS)

Dmitrieva, S.O.; Frontasyeva, M.V.; Dmitriev, A.Yu.; Dmitriev, A.A.

2017-01-01

The work is dedicated to the determination of the origin of archaeological finds from medieval glass using the method of neutron activation analysis (NAA). Among such objects we can discover things not only produced in ancient Russian glassmaking workshops but also imported from Byzantium. The authors substantiate the ancient Russian origin of the medieval glass bracelets of pre-Mongol period, found on the ancient Dubna settlement. The conclusions are based on data on the glass chemical composition obtained as a result of NAA of 10 fragments of bracelets at the IBR-2 reactor, FLNP, JINR.

Gas Chromatography-Mass Spectrometric Analysis of Nematicidal ...

African Journals Online (AJOL)

Purpose: To investigate the chemical composition and nematicidal activity of the essential oil of. Valeriana amurensis ... Methods: The essential oil of V. amurensis roots was obtained by hydrodistillation and analyzed by gas chromatography (GC) ..... Aβ1-40 and Caspase-3 in Alzheimer's disease model rat's brain. J Chin ...

Preliminary characterization of glass fiber sizing

DEFF Research Database (Denmark)

Petersen, Helga Nørgaard; Kusano, Yukihiro; Brøndsted, Povl

2013-01-01

Glass fiber surfaces are treated with sizing during manufacturing. Sizing consists of several components, including a film former and a silane coupling agent that is important for adhesion between glass fibers and a matrix. Although the sizing highly affects the composite interface and thus...... the strength of the composites, little is known about the structure and chemistry of the sizing. A part of sizing was extracted by soxhlet extraction. The fibers were subsequently burned and some fibers were merely burned for analysis of glass fiber and sizing. The results showed that the analyzed fibers had...

Volatility mechanisms of borosilicate glasses and molten glasses of nuclear interest structural effects

International Nuclear Information System (INIS)

Delorme, L.

1998-01-01

This work is devoted to the study of the mechanisms which control the volatility of the reference glass used for the confinement of radioactive waste. It was conducted on simplified compositions, in the SiO 2 -B 2 O 3 -Al 2 O 3 -αNa 2 O-(1-alpha)Li 2 O-CaO system.The structural approach carried out by NMR, from room temperature up to 1500 deg.C, shows a strong increase in the mobility of alkalis above Tg. A rapid exchange between B III and B IV sites near 700 deg.C, and the change of coordination number B IV- B III near 1100 deg.C, also seem to take place. The analysis of the vapor phase, carried out by High Temperature Mass Spectrometry coupled to Knudsen cells, reveals the presence between 780 deg.C and 830 deg.C of NaBO 2 (g), LiBO 2 (g) and Na 2 (BO 2 )2(g). The calculation of the partial pressure of each species shows that the total pressure of simplified glasses is dominated by the contribution of sodium. To study the volatility of glasses at higher temperature, equipment using the Transpiration method was used. The analysis of the deposits indicate the presence at 1060 deg.C of the species quoted previously. The vaporization rate and the vapor density were determined for each composition studied in a saturated state. Thus, we show that the volatility of the reference glass can be simulated by that of a simplified glass. For α=1, the kinetic of vaporization between 1060 deg.C and 1200 deg.C reveals an evaporation from the surface associated with a mechanism of diffusion in the molten glass. This is similar to the volatility of the reference glass at 1060 deg.C. To finally explain these mechanisms on a microscopic basis, we develop a model of molecular interactions. Between 780 deg.C and 830 deg.C, these mechanisms are controlled by a strong attraction between Na 2 O and Li 2 O, which maintains the total vapor pressure on a quasi-constant lever up to α=0.27. (author)

Glass science tutorial: Lecture No. 7, Waste glass technology for Hanford

International Nuclear Information System (INIS)

Kruger, A.A.

1995-07-01

This paper presents the details of the waste glass tutorial session that was held to promote knowledge of waste glass technology and how this can be used at the Hanford Reservation. Topics discussed include: glass properties; statistical approach to glass development; processing properties of nuclear waste glass; glass composition and the effects of composition on durability; model comparisons of free energy of hydration; LLW glass structure; glass crystallization; amorphous phase separation; corrosion of refractories and electrodes in waste glass melters; and glass formulation for maximum waste loading

Corrosion of synthesized glasses and glazes as analogs for nuclear waste glass degradation

International Nuclear Information System (INIS)

Vandiver, P.B.

1994-01-01

Synthesized glasses provide an opportunity to study natural corrosion processes which are intermediate in time span between geological examples of natural glasses, such as obsidians and tektites, and relatively short term laboratory tests lasting a few hours to several decades. In addition, synthesized glasses can usually be tracked to particular archaeological find sites with known dates of production and often burial. Environmental conditions are routinely measured at archaeological sites as a part of the excavation-process, such that information is available on the yearly cycling of temperature and relative humidity, sometimes at the depth at which the artifact was found. Whether the artifacts were excavated in an air enclosure, such as a tomb, or in the soil can also be reconstructed, such that one can determine whether aqueous or atmospheric corrosion was involved in the degradation process. For instance, so-called open-quotes Roman glassclose quotes may span a time period of production of 800 years and a geographical range from Germany to North Africa and from Britain to Afghanistan. One example is the storage during World War II of glass from the British Museum in underground metro stations. Some of these glasses have been in collections for over 100 years. Thus, populations of glasses can be chosen for experimentation which compare variations in bulk composition, dopants, microstructure, heat treatment, ground vs. fire polished surfaces, aqueous vs. atmospheric corrosion, geographic, geological as well as recent storage conditions. Glasses in museums are generally considered to have had their corrosion arrested and be stable because changes in visual appearance are not obvious. However, if we attempt to measure the range of surface water content in these glasses using Fourier transform infrared analysis, a considerable variability is found, as shown

Performance of magneto-optical glass in optical current transducer application

International Nuclear Information System (INIS)

Shen, Yan; Lu, Yunhe; Liu, Zhao; Yu, Xueliang; Zhang, Guoqing; Yu, Wenbin

2015-01-01

First, a theoretical analysis was performed on the effect of temperature on the performance of the sensing element of paramagnetic rare earth-doped magneto-optical glass material that can be used in an optical current transducer application. The effect comprises two aspects: the linear birefringence and the Verdet constant. On this basis, rare earth-doped glass temperature characteristics were studied, and the experimental results indicated that the linear birefringence of rare earth-doped glass increased with increasing temperature, while its magneto-optical sensitivity decreased. Comparative experiments performed for various concentrations of rare earth dopant in the glass revealed that changes in the dopant concentration had no significant effect on the performance of magneto-optical glass. At last, a comparison between rare earth-doped magneto-optical and diamagnetic dense flint glass showed that the sensitivity of the former was six times that of the latter, although the temperature stability of the former was poorer. - Highlights: • Theoretical analysis on the effects of temperature on RE glass. • Rare earth doping leads to higher magneto-optical sensitivity. • The sensitivity of the RE glass is six times that of the dense flint glass

Comprehensive lipidomic analysis of human plasma using multidimensional liquid- and gas-phase separations: Two-dimensional liquid chromatography-mass spectrometry vs. liquid chromatography-trapped-ion-mobility-mass spectrometry.

Science.gov (United States)

Baglai, Anna; Gargano, Andrea F G; Jordens, Jan; Mengerink, Ynze; Honing, Maarten; van der Wal, Sjoerd; Schoenmakers, Peter J

2017-12-29

Recent advancements in separation science have resulted in the commercialization of multidimensional separation systems that provide higher peak capacities and, hence, enable a more-detailed characterization of complex mixtures. In particular, two powerful analytical tools are increasingly used by analytical scientists, namely online comprehensive two-dimensional liquid chromatography (LC×LC, having a second-dimension separation in the liquid phase) and liquid chromatography-ion mobility-spectrometry (LC-IMS, second dimension separation in the gas phase). The goal of the current study was a general assessment of the liquid-chromatography-trapped-ion-mobility-mass spectrometry (LC-TIMS-MS) and comprehensive two-dimensional liquid chromatography-mass spectrometry (LC×LC-MS) platforms for untargeted lipid mapping in human plasma. For the first time trapped-ion-mobility spectrometry (TIMS) was employed for the separation of the major lipid classes and ion-mobility-derived collision-cross-section values were determined for a number of lipid standards. The general effects of a number of influencing parameters have been inspected and possible directions for improvements are discussed. We aimed to provide a general indication and practical guidelines for the analyst to choose an efficient multidimensional separation platform according to the particular requirements of the application. Analysis time, orthogonality, peak capacity, and an indicative measure for the resolving power are discussed as main characteristics for multidimensional separation systems. Copyright © 2017 Elsevier B.V. All rights reserved.

Mechanical failure and glass transition in metallic glasses

International Nuclear Information System (INIS)

Egami, T.

2011-01-01

Research highlights: → We review the recent results of molecular dynamics simulations on metallic glasses. → They show the equivalence of mechanical failure and glass transition. → We discuss the microscopic mechanism behind this equivalence. → We show that the density of defects in metallic glasses is as high as a quarter. → Our concepts about the defect state in glasses need to be changed. - Abstract: The current majority view on the phenomenon of mechanical failure in metallic glasses appears to be that it is caused by the activity of some structural defects, such as free-volumes or shear transformation zones, and the concentration of such defects is small, only of the order of 1%. However, the recent results compel us to revise this view. Through molecular dynamics simulation it has been shown that mechanical failure is the stress-induced glass transition. According to our theory the concentration of the liquid-like sites (defects) is well over 20% at the glass transition. We suggest that the defect concentration in metallic glasses is actually very high, and percolation of such defects causes atomic avalanche and mechanical failure. In this article we discuss the glass transition, mechanical failure and viscosity from such a point of view.

Properties of Formula 127 glass prepared with radioactive zirconia calcine

International Nuclear Information System (INIS)

Staples, B.A.; Pavlica, D.A.; Cole, H.S.

1982-09-01

Formula 127 glass has been developed to immobilize ICPP zirconia calcine. This glass has been prepared remotely on a laboratory scale basis with actual radioactive zirconia calcine retrieved after ten years of storage from Bin Set 2. The aqueous leachability of the glass produced was investigated and compared through application of the MCC-1, MCC-2 and Soxhlet leach tests with that of Formula 127 glass prepared with simulated calcine. The solid state properties of the glasses prepared with actual and simulated calcines were also measured by electron spectroscopy for chemical analysis (ESCA) and scanning electron microscopy energy dispersive x-ray (SEM-EDX). Based on the application of these leaching tests and analysis techniques the properties measured in this study are similar for 127 glass prepared with either simulated or radioactive calcine. 13 figures, 16 tables

Influence of milling process in the surface energy of glass tile frits

International Nuclear Information System (INIS)

Tamayo, A.; Rubio, F.; Otero, J. L.; Rubio, J.

2013-01-01

In this work has been studied the influence of the milling process of two ceramic frits used in the ceramic tile industry. Both glass frits were of similar chemical composition changing SiO 2 by 5% of B 2 O 3 and both of them were water or dry milled. Glass frit surfaces were characterized by FT-IR, Karl-Fischer (K-F) titration and Inverse Gas Chromatography at Infinite Dilution (IGC-ID). By K-F titration it was observed that water milled frits presented 28 and 26 OH groups for 100 A 2 if they do not contain or contain boron, respectively. These surface changes are also observed by IGC-ID. Thus, the glass frit without boron and dry milled presented the highest dispersive surface energy (44 mJ.m - 2) and the less acidic constant (0.13 kJ.mol - 1). Both glass frits are amphoteric with acidic and base surface active sites, and that frit without boron presents the higher basicity. Milling process influences in the acid-base surface characteristics of both frits by increasing the basicity for the one without boron and increasing for the other one. This has been assigned to the different location of hydroxyl groups where the higher interaction is the one that does not contain boron and dry milled as K-F results. (Author)

Crystallization in lead tungsten fluorophosphate glasses

International Nuclear Information System (INIS)

Nardi, R.P.R.D.; Braz, C.E.; Cassanjes, F.C.; Poirier, G.

2014-01-01

The glass forming ability was investigated in the ternary system NaPO 3 -WO 3 -PbF 2 with a constant NaPO 3 /WO 3 ratio of 3/2 and increasing amounts of PbF 2 . It has been found that glass samples can be obtained from PbF 2 contents from 0 mole% to 60 mole%. The most lead fluoride concentrated samples (50% and 60%) were chosen for a crystallization study in order to investigate the possibility of obtaining glass-ceramics containing crystalline lead fluoride. DSC measurements allowed to determine the characteristic temperatures such as Tg, Tx, Tp and Tf. These glass samples were heat-treated near the crystallization peaks observed by thermal analysis. X-ray diffraction results of these heat-treated glasses pointed out that the dominant phase which precipitates from the glass sample containing 50% of PbF 2 is the lead fluorophosphates phase Pb 5 F(PO 4 ) 3 whereas the sample containing 60% of PbF 2 exhibits a preferential crystallization of cubic lead fluoride β-PbF 2 . (author)

Glass fibres reinforced polyester composites degradation monitoring by surface analysis

Energy Technology Data Exchange (ETDEWEB)

Croitoru, Catalin [“Transilvania” University of Brasov, Materials Engineering and Welding Department, Eroilor 29 Str., 500036 Brasov (Romania); Patachia, Silvia, E-mail: st.patachia@unitbv.ro [“Transilvania” University of Brasov, Product Design Environment and Mechatronics Department, Eroilor 29 Str., 500036 Brasov (Romania); Papancea, Adina [“Transilvania” University of Brasov, Product Design Environment and Mechatronics Department, Eroilor 29 Str., 500036 Brasov (Romania); Baltes, Liana; Tierean, Mircea [“Transilvania” University of Brasov, Materials Engineering and Welding Department, Eroilor 29 Str., 500036 Brasov (Romania)

2015-12-15

Highlights: • Glass fibre-reinforced polyester composites surface analysis by photographic method. • The composites are submitted to accelerated ageing by UV irradiation at 254 nm. • The UV irradiation promotes differences in the surface chemistry of the composites. • MB dye is differently adsorbed on surfaces with different degradation degrees. • Good correlation between the colouring degree and surface chemistry. - Abstract: The paper presents a novel method for quantification of the modifications that occur on the surface of different types of gel-coated glass fibre-reinforced polyester composites under artificial UV-ageing at 254 nm. The method implies the adsorption of an ionic dye, namely methylene blue, on the UV-aged composite, and computing the CIELab colour space parameters from the photographic image of the coloured composite's surface. The method significantly enhances the colour differences between the irradiated composites and the reference, in contrast with the non-coloured ones. The colour modifications that occur represent a good indicative of the surface degradation, alteration of surface hydrophily and roughness of the composite and are in good correlation with the ATR-FTIR spectroscopy and optical microscopy results. The proposed method is easier, faster and cheaper than the traditional ones.

Reference document on the long life behavior of nuclear glasses

International Nuclear Information System (INIS)

Godon, N.

2004-01-01

This document exposes the scientific analysis of the operational modelizations concerning the behavior of glasses (C wastes) for the long time storage and for the retrieval or ultimate underground disposal. The scientific approach adopted to establish the behavior of glasses uses a methodology, a strategy and defined approaches, described in this document. The containment glasses specifications, the glass behavior dry or in non saturated open environment, the glass behavior in aqueous environment, predictions models of glasses alteration and elements of validation are also presented. (A.L.B.)

Direction of CRT waste glass processing: Electronics recycling industry communication

International Nuclear Information System (INIS)

Mueller, Julia R.; Boehm, Michael W.; Drummond, Charles

2012-01-01

Highlights: ► Given a large flow rate of CRT glass ∼10% of the panel glass stream will be leaded. ► The supply of CRT waste glass exceeded demand in 2009. ► Recyclers should use UV-light to detect lead oxide during the separation process. ► Recycling market analysis techniques and results are given for CRT glass. ► Academic initiatives and the necessary expansion of novel product markets are discussed. - Abstract: Cathode Ray Tube, CRT, waste glass recycling has plagued glass manufacturers, electronics recyclers and electronics waste policy makers for decades because the total supply of waste glass exceeds demand, and the formulations of CRT glass are ill suited for most reuse options. The solutions are to separate the undesirable components (e.g. lead oxide) in the waste and create demand for new products. Achieving this is no simple feat, however, as there are many obstacles: limited knowledge of waste glass composition; limited automation in the recycling process; transportation of recycled material; and a weak and underdeveloped market. Thus one of the main goals of this paper is to advise electronic glass recyclers on how to best manage a diverse supply of glass waste and successfully market to end users. Further, this paper offers future directions for academic and industry research. To develop the recommendations offered here, a combination of approaches were used: (1) a thorough study of historic trends in CRT glass chemistry; (2) bulk glass collection and analysis of cullet from a large-scale glass recycler; (3) conversations with industry members and a review of potential applications; and (4) evaluation of the economic viability of specific uses for recycled CRT glass. If academia and industry can solve these problems (for example by creating a database of composition organized by manufacturer and glass source) then the reuse of CRT glass can be increased.

Scintillation and optical properties of TiO2-ZnO-Al2O3-B2O3 glasses and glass-ceramics

Science.gov (United States)

Usui, Yuki; Okada, Go; Kawaguchi, Noriaki; Masai, Hirokazu; Yanagida, Takayuki

2018-04-01

13TiO2-xZnO-17Al2O3-(70 - x)B2O3 (x = 17, 26, and 35) glasses were prepared by a melt-quenching method, and the obtained glass samples were heated at temperatures 30 °C above the glass transition temperature of corresponding glass in order to obtain glass-ceramics. The obtained glass-ceramic samples were confirmed to have anatase (x = 17) and rutile (x = 26 and 35) phases from X-ray diffraction analysis. Then, the scintillation and optical properties were evaluated and discussed the difference between the glass-ceramic and glass samples. In the scintillation spectra under X-ray irradiation, a broad emission peak was observed around 450 nm in all the samples, and the new peak around 500 nm appeared in the anatase-precipitated glass-ceramic. The intensities of the glass-ceramic samples were enhanced in comparison with the corresponding glasses because the glass-ceramics includes TiO2 crystallites with defect centers which act as effective emission centers. The scintillation decay curves of the glass and glass-ceramic samples were approximated by one and a sum of two exponential decay functions, respectively. The faster component of glass and glass-ceramic samples would be caused by the host emission, and the slower component of glass-ceramic sample would be ascribed to the emission of Ti3+.

Investigations on vanadium doped glasses

International Nuclear Information System (INIS)

Madhusudana Rao, P.

2013-01-01

The glass samples studied in the present work have been prepared by melt quenching technique. They were prepared by mixing and grinding together by appropriate amounts of Li 2 O - Na 2 O - B 2 O 3 doped with V 2 O 5 in an agate motor before transferring into crucible. The mixtures were heated in an electric furnace at 1225K for 20 mm. The melt was then quenched to room temperature by pouring it on plane brass plate and pressing it with another brass plate. White and yellow coloured glasses have been obtained with good optical quality and high transparency. Finally the vitreous sample were annealed for 3 hrs at 423K to relieve residual internal stress and slowly cooled to room temperature. The polished glasses have been used for XRD, FTIR analysis and for DSC report. The DSC thermo grams for all the glasses were recorded on in the temperature range 50-550℃ with a heating rate of 10℃/min. Electron spin resonance and optical absorption of 20Li 2 O - 10 Na 2 O - (70-X)B 2 O 3 doped with XV 2 O 5 glass system are studied. ESR spectra of V 4+ ions doped in the glass exhibit peak at g =1.98. Spin Hamiltonian parameters are calculated. It was found that these parameters are dependent upon alkali ion concentration in the glass and the VO +2 ion in an octahedral coordination with a tetragonal compression. The physical parameters of all glasses were also evaluated with respect to the composition

Silicate glasses

International Nuclear Information System (INIS)

Lutze, W.

1988-01-01

Vitrification of liquid high-level radioactive wastes has received the greatest attention, world-wide, compared to any other HLW solidification process. The waste form is a borosilicate-based glass. The production of phosphate-based glass has been abandoned in the western world. Only in the Soviet Union are phosphate-based glasses still being developed. Vitrification techniques, equipment and processes and their remote operation have been developed and studied for almost thirty years and have reached a high degree of technical maturity. Industrial demonstration of the vitrification process has been in progress since 1978. This chapter is a survey of world-wide research and development efforts in nuclear waste glasses and its production technology. The principal glasses considered are silicate glasses which contain boron, i.e., borosilicate glasses

Performance Characteristics of Waste Glass Powder Substituting Portland Cement in Mortar Mixtures

Science.gov (United States)

Kara, P.; Csetényi, L. J.; Borosnyói, A.

2016-04-01

In the present work, soda-lime glass cullet (flint, amber, green) and special glass cullet (soda-alkaline earth-silicate glass coming from low pressure mercury-discharge lamp cullet and incandescent light bulb borosilicate glass waste cullet) were ground into fine powders in a laboratory planetary ball mill for 30 minutes. CEM I 42.5N Portland cement was applied in mortar mixtures, substituted with waste glass powder at levels of 20% and 30%. Characterisation and testing of waste glass powders included fineness by laser diffraction particle size analysis, specific surface area by nitrogen adsorption technique, particle density by pycnometry and chemical analysis by X-ray fluorescence spectrophotometry. Compressive strength, early age shrinkage cracking and drying shrinkage tests, heat of hydration of mortars, temperature of hydration, X-ray diffraction analysis and volume stability tests were performed to observe the influence of waste glass powder substitution for Portland cement on physical and engineering properties of mortar mixtures.

Numerical analysis of residual stresses reconstruction for axisymmetric glass components

Science.gov (United States)

Tao, Bo; Xu, Shuang; Yao, Honghui

2018-01-01

A non-destructive measurement method for 3D stress state in a glass cylinder using photoelasticity has been analyzed by simulation in this research. Based on simulated stresses in a glass cylinder, intensity of the cylinder in a circular polariscope can be calculated by Jones calculus. Therefore, the isoclinic angle and optical retardation can be obtained by six steps phase shifting technique. Through the isoclinic angle and optical retardation, the magnitude and distribution of residual stresses inside the glass cylinder in cylindrical coordinate system can be reconstructed. Comparing the reconstructed stresses with numerical simulated stresses, the results verify this non-destructive method can be used to reconstruct the 3D stresses. However, there are some mismatches in axial stress, radial stress and circumferential stress.

High-Level Waste Glass Formulation Model Sensitivity Study 2009 Glass Formulation Model Versus 1996 Glass Formulation Model

International Nuclear Information System (INIS)

Belsher, J.D.; Meinert, F.L.

2009-01-01

This document presents the differences between two HLW glass formulation models (GFM): The 1996 GFM and 2009 GFM. A glass formulation model is a collection of glass property correlations and associated limits, as well as model validity and solubility constraints; it uses the pretreated HLW feed composition to predict the amount and composition of glass forming additives necessary to produce acceptable HLW glass. The 2009 GFM presented in this report was constructed as a nonlinear optimization calculation based on updated glass property data and solubility limits described in PNNL-18501 (2009). Key mission drivers such as the total mass of HLW glass and waste oxide loading are compared between the two glass formulation models. In addition, a sensitivity study was performed within the 2009 GFM to determine the effect of relaxing various constraints on the predicted mass of the HLW glass.

Near-infrared analysis of hydrogen-bonding in glass- and rubber-state amorphous saccharide solids.

Science.gov (United States)

Izutsu, Ken-ichi; Hiyama, Yukio; Yomota, Chikako; Kawanishi, Toru

2009-01-01

Near-infrared (NIR) spectroscopic analysis of noncrystalline polyols and saccharides (e.g., glycerol, sorbitol, maltitol, glucose, sucrose, maltose) was performed at different temperatures (30-80 degrees C) to elucidate the effect of glass transition on molecular interaction. Transmission NIR spectra (4,000-12,000 cm(-1)) of the liquids and cooled-melt amorphous solids showed broad absorption bands that indicate random configuration of molecules. Heating of the samples decreased an intermolecular hydrogen-bonding OH vibration band intensity (6,200-6,500 cm(-1)) with a concomitant increase in a free and intramolecular hydrogen-bonding OH group band (6,600-7,100 cm(-1)). Large reduction of the intermolecular hydrogen-bonding band intensity at temperatures above the glass transition (T(g)) of the individual solids should explain the higher molecular mobility and lower viscosity in the rubber state. Mixing of the polyols with a high T(g) saccharide (maltose) or an inorganic salt (sodium tetraborate) shifted both the glass transition and the inflection point of the hydrogen-bonding band intensity to higher temperatures. The implications of these results for pharmaceutical formulation design and process monitoring (PAT) are discussed.

Introduction to modern liquid chromatography

National Research Council Canada - National Science Library

Snyder, Lloyd R; Kirkland, J. J; Dolan, John W

2010-01-01

"High-performance liquid chromatography (HPLC) is today the leading technique for chemical analysis and related applications, with an ability to separate, analyze, and/or purify virtually any sample...

Ligand exchange chromatography for analysis and preparative separation of tritium-labelled amino acids

International Nuclear Information System (INIS)

Zolotarev, Yu.A.; Zaitsev, D.A.; Penkina, V.I.; Dostavalov, I.N.; Myasoedov, N.F.

1988-01-01

Racemic tritium-labelled amino acids were separated into optical isomers by chromatography on a chiral polyacrylamide sorbent filled with copper ions. The polyacrylamide sorbent is synthesized by Mannich's reaction through the action of formaldehyde and L-phenylalanine upon polyacrylamide Biogel P-4 in an alkali phosphate buffer. Tritium-labelled amino acids are eluted by a weak alkali solution of ammonium carbonate. Data are presented on the ligand exchange chromatography of amino acids depending on the degree to which the sorbent is filled with copper ions and on the eluent concentration. Amino acids are isolated from the eluent on short columns filled with sulfonated cation exchanger in the H + form. HPLC on modified silica gel sorbents is also used for the analysis of tritium-labelled optically active amino acids. Amino acids are eluted by a weakly acidic water-methanol solution containing ammonium acetate. UV and scintillation flow type detectors are used. (author) 7 refs.; 8 figs

Structural study of conventional and bulk metallic glasses during annealing

International Nuclear Information System (INIS)

Pineda, E.; Hidalgo, I.; Bruna, P.; Pradell, T.; Labrador, A.; Crespo, D.

2009-01-01

Metallic glasses with conventional glass-forming ability (Al-Fe-Nd, Fe-Zr-B, Fe-B-Nb compositions) and bulk metallic glasses (Ca-Mg-Cu compositions) were studied by synchrotron X-ray diffraction during annealing throughout glass transition and crystallization temperatures. The analysis of the first diffraction peak position during the annealing process allowed us to follow the free volume change during relaxation and glass transition. The structure factor and the radial distribution function of the glasses were obtained from the X-ray measurements. The structural changes occurred during annealing are analyzed and discussed.

Production of a High-Level Waste Glass from Hanford Waste Samples

International Nuclear Information System (INIS)

Crawford, C.L.; Farrara, D.M.; Ha, B.C.; Bibler, N.E.

1998-09-01

The HLW glass was produced from a HLW sludge slurry (Envelope D Waste), eluate waste streams containing high levels of Cs-137 and Tc-99, solids containing both Sr-90 and transuranics (TRU), and glass-forming chemicals. The eluates and Sr-90/TRU solids were obtained from ion-exchange and precipitation pretreatments, respectively, of other Hanford supernate samples (Envelopes A, B and C Waste). The glass was vitrified by mixing the different waste streams with glass-forming chemicals in platinum/gold crucibles and heating the mixture to 1150 degree C. Resulting glass analyses indicated that the HLW glass waste form composition was close to the target composition. The targeted waste loading of Envelope D sludge solids in the HLW glass was 30.7 wt percent, exclusive of Na and Si oxides. Condensate samples from the off-gas condenser and off-gas dry-ice trap indicated that very little of the radionuclides were volatilized during vitrification. Microstructure analysis of the HLW glass using Scanning Electron Microscopy (SEM) and Energy Dispersive X-Ray Analysis (EDAX) showed what appeared to be iron spinel in the HLW glass. Further X-Ray Diffraction (XRD) analysis confirmed the presence of nickel spinel trevorite (NiFe2O4). These crystals did not degrade the leaching characteristics of the glass. The HLW glass waste form passed leach tests that included a standard 90 degree C Product Consistency Test (PCT) and a modified version of the United States Environmental Protection Agency Toxicity Characteristic Leaching Procedure (TCLP)

Identifying Natural syNergist from Pongamia pinnata Using High-Speed Counter-Current Chromatography Combined with Isobolographic Analysis

Directory of Open Access Journals (Sweden)

Hao Yin

2017-03-01

Full Text Available For identifying the synergistic compounds from Pongamia pinnata, an approach based on high-speed counter-current chromatography (HSCCC combined with isobolographic analysis was designed to detect the synergistic effects in the complex mixture [...

Determination of thermodynamic properties of poly(cyclohexyl methacrylate)by inverse gas chromatography

Institute of Scientific and Technical Information of China (English)

Ismet KAYA; Cigdem Yigit PALA

2014-01-01

In this work,some thermodynamic properties of poly( cyclohexyl methacrylate)were studied by inverse gas chromatography( IGC). For this purpose,the polymeric substance was coated on Chromosorb W and which was filled into a glass column. The retention times(tr)of the probes were determined from the interactions of poly(cyclohexyl methacrylate)with n-pentane,n-hexane,n-heptane,n-octane,n-decane, methanol,ethanol,2-propanol,butanol,acetone,ethyl methyl ketone,benzene,toluene and o-xylene by IGC technique. Then,the specific volume(V0g)was determined for each probe molecule. By using(1/T;lnV0g) graphics,the glass transition temperature of poly( cyclohexyl methacrylate)was found to be 373 K. The adsorp-tion heat under the glass transition temperature(ΔH a ),and partial molar heat of sorption above the glass tran-sition(ΔHS1 ),partial molar free energy of sorption(ΔGS1 )and partial molar entropy of sorption(ΔSS1 )belong-ing to sorption for every probe were calculated. The partial molar heat of mixing at infinite dilution(ΔH∞1 ), partial molar free energy of mixing at infinite dilution(ΔG∞1 ),Flory-Huggins interaction parameter(χ∞12 )and weight fraction activity coefficient(a1/w1)∞ values of polymer-solute systems were calculated at different col-umn temperatures. The solubility parameters(δ2 )of the polymer were obtained by IGC technique.

Determination of thermodynamic properties of poly (cyclohexyl methacrylate) by inverse gas chromatography.

Science.gov (United States)

Kaya, Ismet; Pala, Cigdem Yigit

2014-07-01

In this work, some thermodynamic properties of poly (cyclohexyl methacrylate) were studied by inverse gas chromatography (IGC). For this purpose, the polymeric substance was coated on Chromosorb W and which was filled into a glass column. The retention times (t(r)) of the probes were determined from the interactions of poly (cyclohexyl methacrylate) with n-pentane, n-hexane, n-heptane, n-octane, n-decane, methanol, ethanol, 2-propanol, butanol, acetone, ethyl methyl ketone, benzene, toluene and o-xylene by IGC technique. Then, the specific volume (Vg(0)) was determined for each probe molecule. By using (1/T; lnVg(0)) graphics, the glass transition temperature of poly (cyclohexyl methacrylate) was found to be 373 K. The adsorption heat under the glass transition temperature (deltaH(a)), and partial molar heat of sorption above the glass transition (deltaH1(S)), partial molar free energy of sorption (deltaG1(S)) and partial molar entropy of sorption (deltaS1(S)) belonging to sorption for every probe were calculated. The partial molar heat of mixing at infinite dilution (deltaH1(infinity)), partial molar free energy of mixing at infinite dilution (deltaG1(infinity)), Flory-Huggins interaction parameter (chi12(infinity)) and weight fraction activity coefficient (a1/w1)(infinity) values of polymer-solute systems were calculated at different column temperatures. The solubility parameters (delta2) of the polymer were obtained by IGC technique.

Absorption and emission analysis of RE3+(Sm3+ and Dy3+): lithium boro tellurite glasses.

Science.gov (United States)

Sooraj Hussain, N; Hungerford, G; El-Mallawany, R; Gomes, M J M; Lopes, M A; Ali, Nasar; Santos, J D; Buddhudu, S

2009-06-01

This paper reports on the development and spectral analysis of Sm3+ (1.0%) and Dy3+ (1.0%) doped lithium-boro-tellurite glasses. A bright orange (4G5/2-->6H7/2) along with a red (4G5/2-->6H9/2) and a yellow (4G5/2-->6H5/2) emission transition have been measured from Sm3+ doped lithium-boro-tellurite glass. Both blue (4F9/2-->6H15/2) and yellow (4F9/2-->6H13/2) emission bands have been obtained from Dy3+ glass. From the measured decay profiles, the lifetimes of the emissions of the Sm3+ glass (4G5/2-->6H5/2, 7/2, 9/2 and 11/2) at an excitation of 401 nm have been found to be in the range 0.47-0.81 ms, and with respect to the Dy3+ emissions (4F9/2-->6H15/2 and 13/2), with excitation at 450 nm, are measured to be in the range of 0.302-0.307 ms. Stimulated emission cross-sections (sigmapE) of the measured emission transitions have also been computed and the values are in the range of (0.38-1.20) x 10(-20) cm2 for Sm3+ and for Dy3+ doped lithium-boro-tellurite glass the values are (0.66-1.39) x 10(-20) cm2.

A new bio-active glass ceramic

International Nuclear Information System (INIS)

Shamim, A.; Arif, I.; Suleman, M.; Hussain, K.; Shah, W.A.

1995-01-01

Since 1960 fine ceramics such as alumina have been used side by side with metallic materials for bone and joint replacement. They have high mechanical strength and are free from corrosion problem faced by metals. However they don't bond to the natural living bone and hence are called bio-inactive. This was followed by the development of bio-active glasses and glass-ceramics which bond to the natural bone but have low mechanical strength. In the present work a new bio-active glass-ceramic, based on CaO-SiO/sub 2/-P/sub 2/O/sub 3/-MgO composition, has been developed which has mechanical strength compared to that of a bio-inactive glass ceramic and also bonds strongly to the natural bone. X-ray diffraction analysis reveals wollastanite and apatite phases in the glass ceramic. A new bio-active cement has also been developed which can be used to join broken pieces of bone or by itself at a filler. (author)

Determination of the origin of the medieval glass bracelets discovered in Dubna (Moscow Region, Russia), using the neutron activation analysis

International Nuclear Information System (INIS)

Dmitrieva, S.O.; Frontas'eva, M.V.; Dmitriev, A.Yu.; Dmitriev, A.A.

2016-01-01

The work is dedicated to the determination of the origin of archaeological finds from medieval glass using the method of neutron activation analysis (NAA). Among such objects we can discover things not only produced in ancient Russian glassmaking workshops but also brought from Byzantium. The authors substantiate the ancient Russian origin of the medieval glass bracelets of pre-Mongol period, found on the ancient Dubna settlement. The conclusions are based on the data about the glass chemical composition obtained as a result of NAA of ten fragments of bracelets at the IBR-2 reactor, FLNP, JINR. [ru

Trace analysis in the food and beverage industry by capillary gas chromatography: system performance and maintenance.

Science.gov (United States)

Hayes, M A

1988-04-01

Gas chromatography (GC) is the most widely used analytical technique in the food and beverage industry. This paper addresses the problems of sample preparation and system maintenance to ensure the most sensitive, durable, and efficient results for trace analysis by GC in this industry.

Optimized Synthesis of Foam Glass from Recycled CRT Panel Glass

DEFF Research Database (Denmark)

Petersen, Rasmus Rosenlund; König, Jakob; Yue, Yuanzheng

Most of the panel glass from cathode ray tubes (CRTs) is landfilled today. Instead of landfilling, the panel glass can be turned into new environment-friendly foam glass. Low density foam glass is an effective heat insulating material and can be produced just by using recycle glass and foaming...... additives. In this work we recycle the CRT panel glass to synthesize the foam glass as a crucial component of building and insulating materials. The synthesis conditions such as foaming temperature, duration, glass particle size, type and concentrations of foaming agents, and so on are optimized...... by performing systematic experiments. In particular, the concentration of foaming agents is an important parameter that influences the size of bubbles and the distribution of bubbles throughout the sample. The foam glasses are characterised regarding density and open/closed porosity. Differential scanning...

Interpretation of Coronary Angiograms Recorded Using Google Glass: A Comparative Analysis.

Science.gov (United States)

Duong, Thao; Wosik, Jedrek; Christakopoulos, Georgios E; Martínez Parachini, José Roberto; Karatasakis, Aris; Tarar, Muhammad Nauman Javed; Resendes, Erica; Rangan, Bavana V; Roesle, Michele; Grodin, Jerrold; Abdullah, Shuaib M; Banerjee, Subhash; Brilakis, Emmanouil S

2015-10-01

Google Glass (Google, Inc) is a voice-activated, hands-free, optical head-mounted display device capable of taking pictures, recording videos, and transmitting data via wi-fi. In the present study, we examined the accuracy of coronary angiogram interpretation, recorded using Google Glass. Google Glass was used to record 15 angiograms with 17 major findings and the participants were asked to interpret those recordings on: (1) an iPad (Apple, Inc); or (2) a desktop computer. Interpretation was compared with the original angiograms viewed on a desktop. Ten physicians (2 interventional cardiologists and 8 cardiology fellows) participated. One point was assigned for each correct finding, for a maximum of 17 points. The mean angiogram interpretation score for Google Glass angiogram recordings viewed on an iPad or a desktop vs the original angiograms viewed on a desktop was 14.9 ± 1.1, 15.2 ± 1.8, and 15.9 ± 1.1, respectively (P=.06 between the iPad and the original angiograms, P=.51 between the iPad and recordings viewed on a desktop, and P=.43 between the recordings viewed on a desktop and the original angiograms). In a post-study survey, one of the 10 physicians (10%) was "neutral" with the quality of the recordings using Google Glass, 6 physicians (60%) were "somewhat satisfied," and 3 physicians (30%) were "very satisfied." This small pilot study suggests that the quality of coronary angiogram video recordings obtained using Google Glass may be adequate for recognition of major findings, supporting its expanding use in telemedicine.

Thermomechanical analyses of phenolic foam reinforced with glass fiber mat

International Nuclear Information System (INIS)

Zhou, Jintang; Yao, Zhengjun; Chen, Yongxin; Wei, Dongbo; Wu, Yibing

2013-01-01

Highlights: • Over 10% glass fiber was used to reinforce phenolic foam in the shape of glass fiber mat. • Nucleating agents were used together with glass fiber mat and improved tensile strength of phenolic foam by 215.6%. • Nucleating agents lead to a smaller bubble size of phenolic foam. • The glass transition temperature of phenolic foam remained unchanged during the reinforcement. - Abstract: In this paper, thermomechanical analysis (TMA) and dynamic mechanical analysis were employed to study the properties of phenolic foam reinforced with glass fiber mat. Unreinforced phenolic foam was taken as the control sample. Mechanical tests and scanning electron microscopy were performed to confirm the results of TMA. The results show that glass fiber mat reinforcement improves the mechanical performance of phenolic foam, and nucleating agents improve it further. Phenolic foam reinforced with glass fiber mat has a smaller thermal expansion coefficient compared with unreinforced foam. The storage modulus of the reinforced phenolic foam is also higher than that in unreinforced foam, whereas the loss modulus of the former is lower than that of the latter. The glass transition temperature of the phenolic foam matrix remains unchanged during the reinforcement

Analysis of components from drip tests with ATM-10 glass

International Nuclear Information System (INIS)

Fortner, J.A.; Bates, J.K.; Gerding, T.J.

1996-09-01

Waste package assemblies consisting of actinide-doped West Valley ATM-10 reference glass and sensitized 304L stainless steel have been reacted with simulated repository groundwater using the Unsaturated Test Method. Analyses of surface corrosion and reaction products resulting from tests that were terminated at scheduled intervals between 13 and 52 weeks are reported. Analyses reveal complex interactions between the groundwater, the sensitized stainless steel waste form holder, and the glass. Alteration phases form that consist mainly of smectite clay, brockite, and an amorphous thorium iron titanium silicate, the latter two incorporating thorium, uranium, and possibly transuranics. The results from the terminated tests, combined with data from tests that are still ongoing, will help determine the suitability of glass waste forms in the proposed high-level repository at the Yucca Mountain Site

Recycling of Glass

DEFF Research Database (Denmark)

Christensen, Thomas Højlund; Damgaard, Anders

2011-01-01

Glass is used for many purposes, but in the waste system glass is predominantly found in terms of beverage and food containers with a relatively short lifetime before ending up in the waste. Furthermore there is a large amount of flat glass used in building materials which also ends up in the waste...... system; this glass though has a long lifetime before ending up in the waste. Altogether these product types add up to 82% of the production of the European glass industry (IPCC, 2001). Recycling of glass in terms of cleaning and refilling of bottles as well as the use of broken glass in the production...... of new glass containers is well established in the glass industry. This chapter describes briefly howglass is produced and howwaste glass is recycled in the industry. Quality requirements and use of recycled products are discussed, as are the resource and environmental issues of glass recycling....

Storing of Extracts in Polypropylene Microcentrifuge Tubes Yields Contaminant Peak During Ultra-flow Liquid Chromatographic Analysis.

Science.gov (United States)

Kshirsagar, Parthraj R; Hegde, Harsha; Pai, Sandeep R

2016-05-01

This study was designed to understand the effect of storage in polypropylene microcentrifuge tubes and glass vials during ultra-flow liquid chromatographic (UFLC) analysis. One ml of methanol was placed in polypropylene microcentrifuge tubes (PP material, Autoclavable) and glass vials (Borosilicate) separately for 1, 2, 4, 8, 10, 20, 40, and 80 days intervals stored at -4°C. Contaminant peak was detected in methanol stored in polypropylene microcentrifuge tubes using UFLC analysis. The contaminant peak detected was prominent, sharp detectable at 9.176 ± 0.138 min on a Waters 250-4.6 mm, 4 μ, Nova-Pak C18 column with mobile phase consisting of methanol:water (70:30). It was evident from the study that long-term storage of biological samples prepared using methanol in polypropylene microcentrifuge tubes produce contaminant peak. Further, this may mislead in future reporting an unnatural compound by researchers. Long-term storage of biological samples prepared using methanol in polypropylene microcentrifuge tubes produce contaminant peakContamination peak with higher area under the curve (609993) was obtained in ultra-flow liquid chromatographic run for methanol stored in PP microcentrifuge tubesContamination peak was detected at retention time 9.113 min with a lambda max of 220.38 nm and 300 mAU intensity on the given chromatographic conditionsGlass vials serve better option over PP microcentrifuge tubes for storing biological samples. Abbreviations used: UFLC: Ultra Flow Liquid Chromatography; LC: Liquid Chromatography; MS: Mass spectrometry; AUC: Area Under Curve.

Statistical approach to study of lithium magnesium metaborate glasses

Directory of Open Access Journals (Sweden)

Nedyalkova Miroslava

2017-03-01

Full Text Available Alkali borate glasses and alkaline earth borate glasses are commonly used materials in the field of optoelectronics. Infrared (FTIR and Raman spectroscopy are valuable tools for structural investigation of borate glass networks. The compositional and structural variety of lithium magnesium metaborate glasses is usually determined by traditional instrumental methods. In this study a data set is classified by structural and physicochemical parameters (FTIR, Raman spectra, glass transition temperature-Tg. Characterisation of magnesium containing metaborate glasses by multivariate statistics (hierarchical cluster analysis to reveal potential relationships (similarity or dissimilarity between the type of glasses included in the data set using specific structural features available in the literature is conducted. The clustering of the glass objects indicates a good separation of different magnesium containing borate glass compositions. The grouping of variables concerning Tg and structural data for BO3 and BO4 linkage confirms that BO4/BO3 ratios strongly affect Tg. Additionally, patterns of similarity could be detected not only between the glass composition but also between the features (variables describing the glasses. The proposed approach can be further used as an expert tool for glass properties prediction or fingerprinting (identification of unknown compositions.

1-butanethiol vapor sensing based on gold nanoparticle immobilized on glass slide by digital color analysis

Science.gov (United States)

Shokoufi, Nader; Adeleh, Sara

2017-12-01

We demonstrate that gold nanoparticles (GNPs) immobilized on silanized glass act as an optical sensor that is able to quantify 1-butanethiol vapor. GNPs optical properties in the visible region are dominated by the surface plasmon resonance (SPR). The high affinity between 1-butanethiol and GNPs through Au-s bond leads to change in plasmon feature of GNPs that immobilized on silanized glass and causes absorption decrease at 542 nm in SPR spectrum of GNPs. It can be used as an optical sensor for quantitative detection. In this research, the glass slide surface activated by aminopropyltriethoxysilane (APTES). Spherical GNPs immobilized on silanized glass by silanization agent. The sensor is based on the spectrophotometry and digital color analysis (DCA) through RGB. We monitored R value and linear range 50-700 µM (R 2  =  0.97) with 2.05% relative standard deviation and 26.5 µM value was achieved, for the limit of detection. This method represents advantages of metal gold nanoparticles and solid substrate stability in one package, being inexpensive and low time consuming is another advantage of our method that can be conducted in petrochemical, pharmaceutical industries, and for detection of rotten food in food industries.

Analysis of Influence of Foaming Mixture Components on Structure and Properties of Foam Glass

Science.gov (United States)

Karandashova, N. S.; Goltsman, B. M.; Yatsenko, E. A.

2017-11-01

It is recommended to use high-quality thermal insulation materials to increase the energy efficiency of buildings. One of the best thermal insulation materials is foam glass - durable, porous material that is resistant to almost any effect of substance. Glass foaming is a complex process depending on the foaming mode and the initial mixture composition. This paper discusses the influence of all components of the mixture - glass powder, foaming agent, enveloping material and water - on the foam glass structure. It was determined that glass powder is the basis of the future material. A foaming agent forms a gas phase in the process of thermal decomposition. This aforementioned gas foams the viscous glass mass. The unreacted residue thus changes a colour of the material. The enveloping agent slows the foaming agent decomposition preventing its premature burning out and, in addition, helps to accelerate the sintering of glass particles. The introduction of water reduces the viscosity of the foaming mixture making it evenly distributed and also promotes the formation of water gas that additionally foams the glass mass. The optimal composition for producing the foam glass with the density of 150 kg/m3 is defined according to the results of the research.

Laboratory and field based evaluation of chromatography ...

Science.gov (United States)

The Monitor for AeRosols and GAses in ambient air (MARGA) is an on-line ion-chromatography-based instrument designed for speciation of the inorganic gas and aerosol ammonium-nitrate-sulfate system. Previous work to characterize the performance of the MARGA has been primarily based on field comparison to other measurement methods to evaluate accuracy. While such studies are useful, the underlying reasons for disagreement among methods are not always clear. This study examines aspects of MARGA accuracy and precision specifically related to automated chromatography analysis. Using laboratory standards, analytical accuracy, precision, and method detection limits derived from the MARGA chromatography software are compared to an alternative software package (Chromeleon, Thermo Scientific Dionex). Field measurements are used to further evaluate instrument performance, including the MARGA’s use of an internal LiBr standard to control accuracy. Using gas/aerosol ratios and aerosol neutralization state as a case study, the impact of chromatography on measurement error is assessed. The new generation of on-line chromatography-based gas and particle measurement systems have many advantages, including simultaneous analysis of multiple pollutants. The Monitor for Aerosols and Gases in Ambient Air (MARGA) is such an instrument that is used in North America, Europe, and Asia for atmospheric process studies as well as routine monitoring. While the instrument has been evaluat

Crystallization in lead tungsten fluorophosphate glasses

Energy Technology Data Exchange (ETDEWEB)

Nardi, R.P.R.D.; Braz, C.E.; Cassanjes, F.C.; Poirier, G., E-mail: gael.poirier@unifal-mg.edu.br [Universidade Federal de Alfenas (UNIFAL), Pocos de Caldas, MG (Brazil). Instituto de Ciencia e Tecnologia

2014-07-01

The glass forming ability was investigated in the ternary system NaPO{sub 3}-WO{sub 3}-PbF{sub 2} with a constant NaPO{sub 3}/WO{sub 3} ratio of 3/2 and increasing amounts of PbF{sub 2}. It has been found that glass samples can be obtained from PbF{sub 2} contents from 0 mole% to 60 mole%. The most lead fluoride concentrated samples (50% and 60%) were chosen for a crystallization study in order to investigate the possibility of obtaining glass-ceramics containing crystalline lead fluoride. DSC measurements allowed to determine the characteristic temperatures such as Tg, Tx, Tp and Tf. These glass samples were heat-treated near the crystallization peaks observed by thermal analysis. X-ray diffraction results of these heat-treated glasses pointed out that the dominant phase which precipitates from the glass sample containing 50% of PbF{sub 2} is the lead fluorophosphates phase Pb{sub 5}F(PO{sub 4}){sub 3} whereas the sample containing 60% of PbF{sub 2} exhibits a preferential crystallization of cubic lead fluoride β-PbF{sub 2}. (author)

Isotopic analysis of H2, HD, D2 mixtures and analysis of ortho-para-hydrogen mixtures by gas chromatography

International Nuclear Information System (INIS)

Botter, F.; Perriere, G. de la; Tistchenko, S.

1961-01-01

This communication describes the present situation concerning the possibilities of vapor phase chromatography for the separation and analysis of mixtures of H 2 , HD and D 2 and of ortho- and para-hydrogen mixtures. Separation factors for physical adsorption of the various varieties of hydrogen have been deduced from chromatograms and have also been measured directly with a static method - the agreements is good. (author) [fr

The glass furnace of the 17th Century of Sa Gerreria (Palma, Mallorca): Historical context and preliminary analysis of the materials

International Nuclear Information System (INIS)

Capella Galmes, M. A.; Albero Santacreu, D.

2015-01-01

In this paper the materials of the glass furnace of Sa Gerreria (Palma) dated in the second half of the 17th Century A.D. are analysed. On the one hand, we discuss the available information regarding this glass workshop as well as the raw material management strategies made during the studied period. On the other hand, we focus on the materials produced by this workshop and we carry out a preliminary archaeometrical analysis of the glass lumps, frits and slags recovered as well as some glass pieces by means of scanning electron microscope and X-ray dispersive energy. The final aim is to characterise the chemical composition and the properties of the raw materials used in this workshop as well as to approach some of the technical processes put in practice by the glass makers who inhabited Mallorca during the 17th Century. (Author)

Analysis of polymeric phenolics in red wines using different techniques combined with gel permeation chromatography fractionation.

Science.gov (United States)

Guadalupe, Zenaida; Soldevilla, Alberto; Sáenz-Navajas, María-Pilar; Ayestarán, Belén

2006-04-21

A multiple-step analytical method was developed to improve the analysis of polymeric phenolics in red wines. With a common initial step based on the fractionation of wine phenolics by gel permeation chromatography (GPC), different analytical techniques were used: high-performance liquid chromatography-diode array detection (HPLC-DAD), HPLC-mass spectrometry (MS), capillary zone electrophoresis (CZE) and spectrophotometry. This method proved to be valid for analyzing different families of phenolic compounds, such as monomeric phenolics and their derivatives, polymeric pigments and proanthocyanidins. The analytical characteristics of fractionation by GPC were studied and the method was fully validated, yielding satisfactory statistical results. GPC fractionation substantially improved the analysis of polymeric pigments by CZE, in terms of response, repeatability and reproducibility. It also represented an improvement in the traditional vanillin assay used for proanthocyanidin (PA) quantification. Astringent proanthocyanidins were also analyzed using a simple combined method that allowed these compounds, for which only general indexes were available, to be quantified.

NEW ERBIUM DOPED ANTIMONY GLASSES FOR LASER AND GLASS AMPLIFICATION

Directory of Open Access Journals (Sweden)

B. Tioua

2015-07-01

Full Text Available Because of the special spectroscopic properties of the rare earth ions, rare earth doped glasses are widely used in bulk and fiber lasers or amplifiers. The modelling of lasers and searching for new laser transitions require a precise knowledge of the spectroscopic properties of rare earth ions in different host glasses. In this poster will offer new doped erbium glasses synthesized in silicate crucibles were obtained in the combination Sb2O3-WO3-Na2O. Several properties are measured and correlated with glass compositions. The absorption spectral studies have been performed for erbium doped glasses. The intensities of various absorption bands of the doped glasses are measured and the Judd-Ofelt parameters have been computed. From the theory of Judd-Ofelt, various radiative properties, such as transition probability, branching ratio and radiative life time for various emission levels of these doped glasses have been determined and reported. These results confirm the ability of antimony glasses for glass amplification.

UHPLC: The Greening Face of Liquid Chromatography.

Science.gov (United States)

Cielecka-Piontek, Judyta; Zalewski, Przemysław; Jelińska, Anna; Garbacki, Piotr

2013-01-01

Pharmaceutical analysis based on chromatographic separation is an important part of studies aimed at developing routine quality analysis of drugs. High-performance liquid chromatography (HPLC) is one of the main analytical techniques recommended for drug analysis. Although it meets many criteria vital for analysis, it is time-consuming and uses a relatively high amount of organic solvents compared to other analytical techniques. Recently, Ultra-high-performance liquid chromatography (UHPLC) has been frequently proposed as an alternative to HPLC, which means introducing an environment-friendly approach to drug analysis achieved by reducing the consumption of solvents. It also offers greater chromatographic resolution and higher sensitivity as well as requiring less time due to faster analysis. This review focuses on the basics of UHPLC, compares that technique with HPLC and discusses the possibilities of applying UHPLC for the analysis of different pharmaceuticals and biopharmaceuticals.

Gel chromatography of sup(99m)Tc-labelled compounds

International Nuclear Information System (INIS)

Vilcek, S.; Machan, V.; Kalincak, M.

1976-01-01

The present state of gel chromatography of sup(99m)Tc-labelled compounds is reviewed. Examples are given of gel chromatography for preparing labelled compounds and for quality control analysis and the development of new types of sup(99m)Tc-labelled compounds. The factors which influence the gel chromatography of these compounds are discussed, i.e., the nature of the elution agent, the duration of the contact of the gel and the preparation the gel type, the nature of the labelled compound. The GCS method (gel chromatography scanning) is briefly described. The advantages of gel chromatography as compared with other chromatographic techniques for sup(99m)Tc-labelled compounds are summarized. (author)

Phase transitions and glass transition in a hyperquenched silica–alumina glass

DEFF Research Database (Denmark)

Zhang, Y.F.; Zhao, D.H.; Yue, Yuanzheng

2017-01-01

We investigate phase transitions, glass transition, and dynamic behavior in the hyperquenched 69SiO2–31Al2O3 (mol%) glass (SA glass). Upon reheating, the SA glass exhibits a series of thermal responses. Subsequent to the sub-Tg enthalpy release, the glass undergoes a large jump in isobaric heat...... capacity (ΔCp) during glass transition, implying the fragile nature of the SA glass. The mullite starts to form before the end of glass transition, indicating that the SA glass is extremely unstable against crystallization. After the mullite formation, the remaining glass phase exhibits an increased Tg...... and a suppressed ΔCp. The formation of cristobalite at 1553 K indicates the dominance of silica in the remaining glass matrix. The cristobalite gradually re-melts as the isothermal heat-treatment temperature is raised from 1823 to 1853 K, which is well below the melting point of cristobalite, while the amount...

[Compound preservative and cyclamat determinated by gas chromatography].

Science.gov (United States)

Xin, Ruozhu; Ding, Mei; Zheng, Xianguang; Li, Yajuan

2008-07-01

To establish a gas chromatography method for synchronous determination of six preservatives and cyclamat in cake and pastry. The pre-treatment of complicated compound was finished by dialysis cleaning technology. The interference of the complicated foundation body in the cake and pastry was removed by the best dialysis condition: 2 g/L NaOH of dialysis fluid was dialyzed at the temperature of 25 degrees C for 24h, and the six preservatives and cyclamat (sorbic acid, benzoic acid, dehydroacetic acid, ethylparabenum, propylparabenum, butylparabenun and sodium cyclamate) were synchronously seperated by 60-80 mesh Chromosorb WAW DMCS glass packing column of intercoated 5% DEGS + 1% H3 PO4. The seven components in the sample had a good lining relation at the concentration 100 -5000 mg/L when the external standard method was used, and their correlation coefficients were 0.9993-0.9998, and their average recovery rates were 87.5%-101.9%, and their relative standard deviations were 0.64%-3.3%, and detection limits were 1.1-8.8 mg/L. This method could be used to quickly analyse the compound preservatives of the large batch cake and pastry through the common gas chromatography and packed column and this method was simple, accurate and quick.

[Analysis of phthalates in plastic food-packaging bags by thin layer chromatography].

Science.gov (United States)

Chen, Hui; Wang, Yuan; Zhu, Ruohua

2006-01-01

The method for simultaneous determination of four phthalates, namely dimethyl phthalate (DMP), diethyl phthalate (DEP), di-n-butyl phthalate (DBP) and di (2-ethylhexyl) phthalate (DEHP) in plastic food-packaging bags by thin layer chromatography (TLC) was developed. The plastic food-packaging bags were extracted with ethanol by ultrasonication, then the mixture was filtrated through membrane (0.45 microm). The mixture of ethyl acetate-anhydrous ether-isooctane (1 : 4 : 15, v/v) was used as developing agent on the TLC silica gel plate for development. The filtered liquid was spotted on the TLC plate dealt by acetone, and detected with scanning wavelength of 275 nm and reference wavelength of 340 nm. The qualitative analysis of the phthalates was performed using the R(f) values of the chromatogram. The quantitative analysis was performed with external standard method. Good linearities were obtained for DMP, DEP, DBP and DEHP. The detection limits were 2.1 ng for DMP, 2.4 ng for DEP, 3.4 ng for DBP and 4.0 ng for DEHP. The relative standard deviations (RSDs) of the four phthalates were 2.8% - 3.5%. The recoveries of the four phthalate standards in real sample were 78.58% - 111.04%. The method presented has the advantages of high precision, high sensitivity, small sample size, and simple pretreatment . The method was used to detect the four phthalates in the food-packaging bags. The contents in real samples were close to the results by gas chromatography.

Analysis of catecholamines in urine by unique LC/MS suitable ion-pairing chromatography.

Science.gov (United States)

Bergmann, Marianne L; Sadjadi, Seyed; Schmedes, Anne

2017-07-01

The catecholamines, epinephrine (E) and norepinephrine (NE) are small polar, hydrophilic molecules, posing significant challenges to liquid chromatography - tandem mass spectrometry (LC-MS/MS) method development. Specifically, these compounds show little retention on conventional reversed-phase liquid chromatography columns. This work presents development and validation of an LC-MS/MS method for determining catecholamines in urine, based on a new approach to ion-pairing chromatography (IPC), in which the ion-pairing reagent (IPR), 1-Heptane Sulfonic Acid (HSA), is added to the extracted samples instead of the mobile phases. A Hamilton STARlet workstation carried out the solid phase extraction of urine samples. The extracted samples were diluted with 60mmol/L HSA and injected on a Kinetex core-shell biphenyl column with conventional LC-MS/MS suitable mobile phases. Chromatographic separation of E and NE was achieved successfully with very stable retention times (RT). In 484 injections, the RTs were steady with a CV of less than ±4%. Furthermore, HSA was separated from E and NE, allowing HSA to be diverted to waste instead of entering the mass spectrometer ion chamber. The method was validated with good analytical performance, and even though the analysis for urinary catecholamines is increasingly being replaced by plasma free metanephrines in diagnosing pheochromocytomas, this work represents the application of a new analytical technique that can be transferred to other small polar molecules, that are difficult to chromatograph on traditional reversed phase columns. Copyright © 2017 Elsevier B.V. All rights reserved.

Atomic Force Microscope Mediated Chromatography

Science.gov (United States)

Anderson, Mark S.

2013-01-01

The atomic force microscope (AFM) is used to inject a sample, provide shear-driven liquid flow over a functionalized substrate, and detect separated components. This is demonstrated using lipophilic dyes and normal phase chromatography. A significant reduction in both size and separation time scales is achieved with a 25-micron-length column scale, and one-second separation times. The approach has general applications to trace chemical and microfluidic analysis. The AFM is now a common tool for ultra-microscopy and nanotechnology. It has also been demonstrated to provide a number of microfluidic functions necessary for miniaturized chromatography. These include injection of sub-femtoliter samples, fluidic switching, and sheardriven pumping. The AFM probe tip can be used to selectively remove surface layers for subsequent microchemical analysis using infrared and tip-enhanced Raman spectroscopy. With its ability to image individual atoms, the AFM is a remarkably sensitive detector that can be used to detect separated components. These diverse functional components of microfluidic manipulation have been combined in this work to demonstrate AFM mediated chromatography. AFM mediated chromatography uses channel-less, shear-driven pumping. This is demonstrated with a thin, aluminum oxide substrate and a non-polar solvent system to separate a mixture of lipophilic dyes. In conventional chromatographic terms, this is analogous to thin-layer chromatography using normal phase alumina substrate with sheardriven pumping provided by the AFM tip-cantilever mechanism. The AFM detection of separated components is accomplished by exploiting the variation in the localized friction of the separated components. The AFM tip-cantilever provides the mechanism for producing shear-induced flows and rapid pumping. Shear-driven chromatography (SDC) is a relatively new concept that overcomes the speed and miniaturization limitations of conventional liquid chromatography. SDC is based on a

Cromatografia unificada Unified chromatography

Directory of Open Access Journals (Sweden)

Carin von Mühlen

2004-10-01

Full Text Available The scope of this study encompasses an overview of the principles of unified chromatography as well as the principles of chromatographic techniques as applied to unified systems, which include gas chromatography, liquid chromatography, supercritical fluid chromatography, high temperature and high pressure liquid chromatography, micro-liquid chromatography, enhanced fluidity chromatography, and solvating gas chromatography. Theoretical considerations and individual instrumental parameters such as mobile phase, sample introduction system, columns, and detection system are also discussed. Future applications of this separation approach are discussed.

Properties of Desert Sand and CMAS Glass

Science.gov (United States)

Bansal, Narottam P.; Choi, Sung R.

2014-01-01

As-received desert sand from a Middle East country has been characterized for its phase composition and thermal stability. X-ray diffraction analysis showed the presence of quartz (SiO2), calcite (CaCO3), gypsum (CaSO4.2H2O), and NaAlSi3O8 phases in as-received desert sand and showed weight loss of approx. 35 percent due to decomposition of CaCO3 and CaSO4.2H2O when heated to 1400 C. A batch of as-received desert sand was melted into calcium magnesium aluminosilicate (CMAS) glass at approx. 1500 C. From inductively coupled plasma-atomic emission spectrometry, chemical composition of the CMAS glass was analyzed to be 27.8CaO-4MgO-5Al2O3-61.6SiO2-0.6Fe2O3-1K2O (mole percent). Various physical, thermal and mechanical properties of the glass have been evaluated. Bulk density of CMAS glass was 2.69 g/cc, Young's modulus 92 GPa, Shear modulus 36 GPa, Poisson's ratio 0.28, dilatometric glass transition temperature (T (sub g)) 706 C, softening point (T (sub d)) 764 C, Vickers microhardness 6.3 +/- 0.4 GPa, indentation fracture toughness 0.75 +/- 0.15 MPa.m (sup 1/2), and coefficient of thermal expansion (CTE) 9.8 x 10 (exp -6)/degC in the temperature range 25 to 700 C. Temperature dependence of viscosity has also been estimated from various reference points of the CMAS glass using the Vogel-Fulcher-Tamman (VFT) equation. The glass remained amorphous after heat treating at 850 C for 10 hr but crystallized into CaSiO3 and Ca-Mg-Al silicate phases at 900 C or higher temperatures. Crystallization kinetics of the CMAS glass has also been investigated by differential thermal analysis (DTA). Activation energies for the crystallization of two different phases in the glass were calculated to be 403 and 483 kJ/mol, respectively.

Structural analysis of fluorine-containing bioactive glass nanoparticles synthesized by sol-gel route assisted by ultrasound energy.

Science.gov (United States)

Lins, Carolina E C; Oliveira, Agda A R; Gonzalez, Ismael; Macedo, Waldemar A A; Pereira, Marivalda M

2018-01-01

In the last decades, studies about the specific effects of bioactive glass on remineralization of dentin were the focus of attention, due to their excellent regenerative properties in mineralized tissues. The incorporation of Fluorine in bioactive glass nanoparticles may result in the formation of fluorapatite (FAP), which is chemically more stable than hydroxyapatite or carbonated hydroxyapatite, and therefore is of interest for dental applications. The aim of this study was to synthesize and characterize a new system of Fluorine-containing bioactive glass nanoparticles (BGNPF). A sol-gel route assisted by ultrasound was used for the synthesis of BGNPF. The particles obtained were characterized by scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), atomic force microscopy (AFM), X-ray diffraction (XRD), dynamic light scattering (DLS), nitrogen adsorption, and X-ray photoelectron spectroscopy (XPS). SEM micrographs showed that the particles are quite uniform spherical nanostructures, occurring agglomeration or partial sinterization of the particulate system after heat treatment. XRD and XPS analysis results suggest the formation of fluorapatite crystals embedded within the matrix of the bioactive glass nanoparticles. © 2017 Wiley Periodicals, Inc. J Biomed Mater Res Part B: Appl Biomater, 106B: 360-366, 2018. © 2017 Wiley Periodicals, Inc.

Liquid -to-glass transition in bulk glass-forming Cu55-xZr45Agx alloys using molecular dynamic simulations

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Celtek M.

2011-05-01

Full Text Available We report results from molecular dynamics (MD studies concerning the microscopic structure of the ternary, bulk metallic glass-forming Cu55-x Zr45Agx (x=0,10,20 alloys using tight-binding potentials. Understanding of the nature of Glass Forming Ability (GFA of studied alloys, GFA parameters, glass transition temperature (T-g, melting temperature (T-m, reduced glass transition temperature (T-g/T-m, the supercooled liquid region and other parameters were simulated and compared with experiments. The computed pair distribution functions reproduce well experimental x-ray data of Inoue and co-workers. Structure analysis of the Cu-Zr-Ag alloy based on MD simulation will be also presented

Quantitative chromatography in the analysis of labelled compounds 1. Quantitative paper chromotography of amino acids by A spot comparison technique

International Nuclear Information System (INIS)

Barakat, M.F.; Farag, A.N.; El-Gharbawy, A.A.

1974-01-01

For the determination of the specific activity of labelled compounds separated by paper sheet chromatography, it was found essential to perfect the quantitative aspect of the paper chromatographic technique. Actually, so far paper chromatography has been used as a separation tool mainly and its use in quantification of the separated materials is by far less studied. In the present work, the quantitative analysis of amino acids by paper sheet chromatography has been carried out by methods, depending on the use of the relative spot area values for correcting the experimental data obtained. The results obtained were good and reproducible. The main advantage of the proposed technique is its extreme simplicity. No complicated equipment of procedures are necessary

Applications of hydrophilic interaction chromatography to amino acids, peptides, and proteins.

Science.gov (United States)

Periat, Aurélie; Krull, Ira S; Guillarme, Davy

2015-02-01

This review summarizes the recent advances in the analysis of amino acids, peptides, and proteins using hydrophilic interaction chromatography. Various reports demonstrate the successful analysis of amino acids under such conditions. However, a baseline resolution of the 20 natural amino acids has not yet been published and for this reason, there is often a need to use mass spectrometry for detection to further improve selectivity. Hydrophilic interaction chromatography is also recognized as a powerful technique for peptide analysis, and there are a lot of papers showing its applicability for proteomic applications (peptide mapping). It is expected that its use for peptide mapping will continue to grow in the future, particularly because this analytical strategy can be combined with reversed-phase liquid chromatography, in a two-dimensional setup, to reach very high resolving power. Finally, the interest in hydrophilic interaction chromatography for intact proteins analysis is less evident due to possible solubility issues and a lack of suitable hydrophilic interaction chromatography stationary phases. To date, it has been successfully employed only for the characterization of membrane proteins, histones, and the separation of glycosylated isoforms of an intact glycoprotein. From our point of view, the number of hydrophilic interaction chromatography columns compatible with intact proteins (higher upper temperature limit, large pore size, etc.) is still too limited. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Strength on cut edge and ground edge glass beams with the failure analysis method

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Stefano Agnetti

2013-10-01

Full Text Available The aim of this work is the study of the effect of the finishing of the edge of glass when it has a structural function. Experimental investigations carried out for glass specimens are presented. Various series of annealed glass beam were tested, with cut edge and with ground edge. The glass specimens are tested in four-point bending performing flaw detection on the tested specimens after failure, in order to determine glass strength. As a result, bending strength values are obtained for each specimen. Determining some physical parameter as the depth of the flaw and the mirror radius of the fracture, after the failure of a glass element, it could be possible to calculate the failure strength of that.The experimental results were analyzed with the LEFM theory and the glass strength was analyzed with a statistical study using two-parameter Weibull distribution fitting quite well the failure stress data. The results obtained constitute a validation of the theoretical models and show the influence of the edge processing on the failure strength of the glass. Furthermore, series with different sizes were tested in order to evaluate the size effect.

Proposed method for determining the thickness of glass in solar collector panels

Science.gov (United States)

Moore, D. M.

1980-01-01

An analytical method was developed for determining the minimum thickness for simply supported, rectangular glass plates subjected to uniform normal pressure environmental loads such as wind, earthquake, snow, and deadweight. The method consists of comparing an analytical prediction of the stress in the glass panel to a glass breakage stress determined from fracture mechanics considerations. Based on extensive analysis using the nonlinear finite element structural analysis program ARGUS, design curves for the structural analysis of simply supported rectangular plates were developed. These curves yield the center deflection, center stress and corner stress as a function of a dimensionless parameter describing the load intensity. A method of estimating the glass breakage stress as a function of a specified failure rate, degree of glass temper, design life, load duration time, and panel size is also presented.

Spherical 2+p spin-glass model: An exactly solvable model for glass to spin-glass transition

International Nuclear Information System (INIS)

Crisanti, A.; Leuzzi, L.

2004-01-01

We present the full phase diagram of the spherical 2+p spin-glass model with p≥4. The main outcome is the presence of a phase with both properties of full replica symmetry breaking phases of discrete models, e.g., the Sherrington-Kirkpatrick model, and those of one replica symmetry breaking. This phase has a finite complexity which leads to different dynamic and static properties. The phase diagram is rich enough to allow the study of different kinds of glass to spin glass and spin glass to spin glass phase transitions

Glass binder development for a glass-bonded sodalite ceramic waste form

International Nuclear Information System (INIS)

Riley, Brian J.; Vienna, John D.; Frank, Steven M.; Kroll, Jared O.; Peterson, Jacob A.

2017-01-01

This paper discusses work to develop Na_2O-B_2O_3-SiO_2 glass binders for immobilizing LiCl-KCl eutectic salt waste in a glass-bonded sodalite waste form following electrochemical reprocessing of used metallic nuclear fuel. In this paper, five new glasses with ~20 mass% Na_2O were designed to generate waste forms with high sodalite. The glasses were then used to produce ceramic waste forms with a surrogate salt waste. The waste forms made using these new glasses were formulated to generate more sodalite than those made with previous baseline glasses for this type of waste. The coefficients of thermal expansion for the glass phase in the glass-bonded sodalite waste forms made with the new binder glasses were closer to the sodalite phase in the critical temperature region near and below the glass transition temperature than previous binder glasses used. Finally, these improvements should result in lower probability of cracking in the full-scale monolithic ceramic waste form, leading to better long-term chemical durability.

Quantitative analysis of benzodiazepines in vitreous humor by high-performance liquid chromatography

Science.gov (United States)

Bazmi, Elham; Behnoush, Behnam; Akhgari, Maryam; Bahmanabadi, Leila

2016-01-01

Objective: Benzodiazepines are frequently screened drugs in emergency toxicology, drugs of abuse testing, and in forensic cases. As the variations of benzodiazepines concentrations in biological samples during bleeding, postmortem changes, and redistribution could be biasing forensic medicine examinations, hence selecting a suitable sample and a validated accurate method is essential for the quantitative analysis of these main drug categories. The aim of this study was to develop a valid method for the determination of four benzodiazepines (flurazepam, lorazepam, alprazolam, and diazepam) in vitreous humor using liquid–liquid extraction and high-performance liquid chromatography. Methods: Sample preparation was carried out using liquid–liquid extraction with n-hexane: ethyl acetate and subsequent detection by high-performance liquid chromatography method coupled to diode array detector. This method was applied to quantify benzodiazepines in 21 authentic vitreous humor samples. Linear curve for each drug was obtained within the range of 30–3000 ng/mL with coefficient of correlation higher than 0.99. Results: The limit of detection and quantitation were 30 and 100 ng/mL respectively for four drugs. The method showed an appropriate intra- and inter-day precision (coefficient of variation forensic toxicology laboratory. PMID:27635251

Study of structural, electrical, and dielectric properties of phosphate-borate glasses and glass-ceramics

Energy Technology Data Exchange (ETDEWEB)

Melo, B. M. G.; Graça, M. P. F., E-mail: mpfg@ua.pt; Prezas, P. R.; Valente, M. A. [Physics Department (I3N), Aveiro University, Campus Universitário de Santiago, Aveiro (Portugal); Almeida, A. F.; Freire, F. N. A. [Mechanics Engineering Department, Ceará Federal University, Fortaleza (Brazil); Bih, L. [Equipe Physico-Chimie la Matière Condensée, Faculté des Sciences de Meknès, Meknès (Morocco)

2016-08-07

In this work, phosphate-borate based glasses with molar composition 20.7P{sub 2}O{sub 5}–17.2Nb{sub 2}O{sub 5}–13.8WO{sub 3}–34.5A{sub 2}O–13.8B{sub 2}O{sub 3}, where A = Li, Na, and K, were prepared by the melt quenching technique. The as-prepared glasses were heat-treated in air at 800 °C for 4 h, which led to the formation of glass-ceramics. These high chemical and thermal stability glasses are good candidates for several applications such as fast ionic conductors, semiconductors, photonic materials, electrolytes, hermetic seals, rare-earth ion host solid lasers, and biomedical materials. The present work endorses the analysis of the electrical conductivity of the as-grown samples, and also the electrical, dielectric, and structural changes established by the heat-treatment process. The structure of the samples was analyzed using X-Ray powder Diffraction (XRD), Raman spectroscopy, and density measurements. Both XRD and Raman analysis confirmed crystals formation through the heat-treatment process. The electrical ac and dc conductivities, σ{sub ac} and σ{sub dc}, respectively, and impedance spectroscopy measurements as function of the temperature, varying from 200 to 380 K, were investigated for the as-grown and heat-treated samples. The impedance spectroscopy was measured in the frequency range of 100 Hz–1 MHz.

Using physical properties of molten glass to estimate glass composition

International Nuclear Information System (INIS)

Choi, Kwan Sik; Yang, Kyoung Hwa; Park, Jong Kil

1997-01-01

A vitrification process is under development in KEPRI for the treatment of low-and medium-level radioactive waste. Although the project is for developing and building Vitrification Pilot Plant in Korea, one of KEPRI's concerns is the quality control of the vitrified glass. This paper discusses a methodology for the estimation of glass composition by on-line measurement of molten glass properties, which could be applied to the plant for real-time quality control of the glass product. By remotely measuring viscosity and density of the molten glass, the glass characteristics such as composition can be estimated and eventually controlled. For this purpose, using the database of glass composition vs. physical properties in isothermal three-component system of SiO 2 -Na 2 O-B 2 O 3 , a software TERNARY has been developed which determines the glass composition by using two known physical properties (e.g. density and viscosity)

Liquid chromatography - mass spectrometry analysis of pharmaceuticals

International Nuclear Information System (INIS)

Macasek, F.

2003-01-01

The drugs represent mostly non-volatile and thermally labile solutes, often available only in small amounts like it is in case of radiopharmaceuticals. Therefor, the favourable separation techniques for such compounds are HPLC, capillary electrophoresis and also TLC 1. Liquid chromatography with mass spectrometric detector (LC/MS) is especially powerful for their microanalysis. Mass spectrometry separating the ions in high vacuum was presumably used as detector for gas chromatography effluent but the on-line coupling with liquid eluant flow 0.1-1 mL/min is far more challenging. New types of ion sources were constructed for simultaneous removal of solvent and ionisation of solutes at atmospheric pressure (API). At present, a relatively wide choice of successfully designed commercial equipment is available either for small organic molecules and larger biomolecules (Perkin-Elmer, Agilent, Jeol, Bruker Daltonics, ThermoQuest, Shimadzu). The features of the LC/MS systems are presented. LC/MS as a new quality control tool for [F-18]fluorodeoxyglucose (FDG) radiopharmaceutical, which has became the most spread radiopharmaceutical for positron emission tomography (PET), was proposed. Other applications of the LC/MS are reviewed. (author)

Measurement of edge residual stresses in glass by the phase-shifting method

Science.gov (United States)

Ajovalasit, A.; Petrucci, G.; Scafidi, M.

2011-05-01

Control and measurement of residual stress in glass is of great importance in the industrial field. Since glass is a birefringent material, the residual stress analysis is based mainly on the photoelastic method. This paper considers two methods of automated analysis of membrane residual stress in glass sheets, based on the phase-shifting concept in monochromatic light. In particular these methods are the automated versions of goniometric compensation methods of Tardy and Sénarmont. The proposed methods can effectively replace manual methods of compensation (goniometric compensation of Tardy and Sénarmont, Babinet and Babinet-Soleil compensators) provided by current standards on the analysis of residual stresses in glasses.

Analysis of the DWPF glass pouring system using neural networks

International Nuclear Information System (INIS)

Calloway, T.B. Jr.; Jantzen, C.M.

1997-01-01

Neural networks were used to determine the sensitivity of 39 selected Melter/Melter Off Gas and Melter Feed System process parameters as related to the Defense Waste Processing Facility (DWPF) Melter Pour Spout Pressure during the overall analysis and resolution of the DWPF glass production and pouring issues. Two different commercial neural network software packages were used for this analysis. Models were developed and used to determine the critical parameters which accurately describe the DWPF Pour Spout Pressure. The model created using a low-end software package has a root mean square error of ± 0.35 inwc ( 2 = 0.77) with respect to the plant data used to validate and test the model. The model created using a high-end software package has a R 2 = 0.97 with respect to the plant data used to validate and test the model. The models developed for this application identified the key process parameters which contribute to the control of the DWPF Melter Pour Spout pressure during glass pouring operations. The relative contribution and ranking of the selected parameters was determined using the modeling software. Neural network computing software was determined to be a cost-effective software tool for process engineers performing troubleshooting and system performance monitoring activities. In remote high-level waste processing environments, neural network software is especially useful as a replacement for sensors which have failed and are costly to replace. The software can be used to accurately model critical remotely installed plant instrumentation. When the instrumentation fails, the software can be used to provide a soft sensor to replace the actual sensor, thereby decreasing the overall operating cost. Additionally, neural network software tools require very little training and are especially useful in mining or selecting critical variables from the vast amounts of data collected from process computers

The influence of gamma radiation on the molecular weight and glass transition of PLLA and HAp/PLLA nanocomposite

International Nuclear Information System (INIS)

Milicevic, D.; Trifunovic, S.; Dojcilovic, J.; Ignjatovic, N.; Suljovrujic, E.

2010-01-01

The influence of gamma radiation on the molecular weight and glass transition behaviour of poly-L-lactide (PLLA) and hydroxyapatite/poly-L-lactide (HAp/PLLA) nanocomposite has been studied. Since PLLA exposed to high-energy radiation in the presence of air is prone to chain scission reactions and large degradation, changes in molecular weight were obtained by gel permeation chromatography (GPC). Alterations in the glass transition behaviour were investigated by differential scanning calorimetry (DSC). The apparent activation energy (ΔH*) for glass transition was determined on the basis of the heating rate dependence of the glass transition temperature (T g ). Our findings support the fact that chain scission is the main reason for the decrease of T g and ΔH* with the absorbed dose. Furthermore, more intensive chain scission degradation of PLLA was observed in HAp/PLLA and can only be ascribed to the presence of HAp nanoparticles. Consequently, initial differences in the glass transition temperature and/or apparent activation energy of PLLA and HAp/PLLA became more pronounced with absorbed dose. This study reveals that radiation-induced changes in molecular weight and glass transition temperature occur in a predictable and fairly accurate manner. Therefore, gamma radiation can be used not only for sterilization but also for tailoring desirable end-use properties of these biomaterials.

Clinical analysis of asthenopia caused by wearing inappropriate glasses in college students

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Li Wang

2015-01-01

Full Text Available AIM: To proposed control measures by exploring visual fatigue caused by college students wearing inappropriate glasses.METHODS: A total of 124 cases of asthenopia patients underwent optometry students audition, checked the original spectacles; TOPCON-CL100 computer center was used to checked the original mirror glasses(glasses, the distance between the optical center; with near vision as the standard examination table nearly with vergence and regulation near point, and checked the visual function. RESULTS: All 124 cases(248 eyeshad refractive errors, 77% were spherical mirror and 69% column mirror with error ≥±0.50D, and the pupil center distance from the lens had significant difference(U=5.27, PCONCLUSION: Students wearing inappropriate spectacle asthenopia is caused by one of the main scientific wearing glasses can effectively control asthenopia.

Size-exclusion chromatography using core-shell particles.

Science.gov (United States)

Pirok, Bob W J; Breuer, Pascal; Hoppe, Serafine J M; Chitty, Mike; Welch, Emmet; Farkas, Tivadar; van der Wal, Sjoerd; Peters, Ron; Schoenmakers, Peter J

2017-02-24

Size-exclusion chromatography (SEC) is an indispensable technique for the separation of high-molecular-weight analytes and for determining molar-mass distributions. The potential application of SEC as second-dimension separation in comprehensive two-dimensional liquid chromatography demands very short analysis times. Liquid chromatography benefits from the advent of highly efficient core-shell packing materials, but because of the reduced total pore volume these materials have so far not been explored in SEC. The feasibility of using core-shell particles in SEC has been investigated and contemporary core-shell materials were compared with conventional packing materials for SEC. Columns packed with very small core-shell particles showed excellent resolution in specific molar-mass ranges, depending on the pore size. The analysis times were about an order of magnitude shorter than what could be achieved using conventional SEC columns. Copyright © 2016 Elsevier B.V. All rights reserved.

Ionic liquids as silica deactivating agents in gas chromatography for direct analysis of primary amines in water

NARCIS (Netherlands)

Krzyzaniak, A.; Weggemans, W.M.A.; Schuur, B.; Haan, de A.B.

2011-01-01

Analysis of primary amines in aqueous samples remains a challenging analytical issue. The preferred approach by gas chromatography is hampered by interactions of free silanol groups with the highly reactive amine groups, resulting in inconsistent measurements. Here, we report a method for direct

Ionic liquids as silica deactivating agents in gas chromatography for direct analysis or primary amines in water

NARCIS (Netherlands)

Krzyzaniak, A.; Weggemans, W.; Schuur, Boelo; de Haan, A.B.

2011-01-01

Analysis of primary amines in aqueous samples remains a challenging analytical issue. The preferred approach by gas chromatography is hampered by interactions of free silanol groups with the highly reactive amine groups, resulting in inconsistent measurements. Here, we report a method for direct

Mechanical properties of zirconia reinforced lithium silicate glass-ceramic.

Science.gov (United States)

Elsaka, Shaymaa E; Elnaghy, Amr M

2016-07-01

The aim of this study was to assess the mechanical properties of recently introduced zirconia reinforced lithium silicate glass-ceramic. Two types of CAD/CAM glass-ceramics (Vita Suprinity (VS); zirconia reinforced lithium silicate and IPS e.max CAD (IC); lithium disilicate) were used. Fracture toughness, flexural strength, elastic modulus, hardness, brittleness index, and microstructures were evaluated. Data were analyzed using independent t tests. Weibull analysis of flexural strength data was also performed. VS had significantly higher fracture toughness (2.31±0.17MPam(0.5)), flexural strength (443.63±38.90MPa), elastic modulus (70.44±1.97GPa), and hardness (6.53±0.49GPa) than IC (Pglass-ceramic revealed significantly a higher brittleness index (2.84±0.26μm(-1/2)) (lower machinability) than IC glass-ceramic (Pglass-ceramic revealed a lower probability of failure and a higher strength than IC glass-ceramic according to Weibull analysis. The VS zirconia reinforced lithium silicate glass-ceramic revealed higher mechanical properties compared with IC lithium disilicate glass-ceramic. Copyright © 2016 The Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Cross-craft interactions between metal and glass working: slag additions to early Anglo-Saxon red glass

Science.gov (United States)

Peake, James R. N.; Freestone, Ian C.

Opaque red glass has been extensively studied over the years, but its compositional complexity and variability means that the way in which it was manufactured is still not fully understood. Previous studies have suggested the use of metallurgical by-products in its manufacture, but until now the evidence has been limited. SEM-EDS analysis of glass beads from the early Anglo-Saxon cemetery complex at Eriswell, southeast England, has provided further insights into the production and technology of opaque red glass, which could only have been possible through invasive sampling. The matrix of the red glasses contains angular particles of slag, the main phases of which typically correspond to either fayalite (Fe2SiO4) or kirschsteinite (CaFeSiO4), orthosilicate (olivine-type) minerals characteristic of some copper- and iron-smelting slags. This material appears to have been added in part as a reducing agent, to promote the precipitation of sub-micrometer particles of the colorant phase, copper metal. Its use represents a sophisticated, if empirical, understanding of materials and can only have resulted through deliberate experimentation with metallurgical by-products by early glass workers. Slag also seems to have been added as a source of iron to colour `black' glass. The compositions of the opaque red glasses appear to be strongly paralleled by Merovingian beads from northern Europe and Anglo-Saxon beads from elsewhere in England, suggesting that this technology is likely to have been quite widespread.

New insights into liquid chromatography for more eco-friendly analysis of pharmaceuticals.

Science.gov (United States)

Shaaban, Heba

2016-10-01

Greening the analytical methods used for analysis of pharmaceuticals has been receiving great interest aimed at eliminating or minimizing the amount of organic solvents consumed daily worldwide without loss in chromatographic performance. Traditional analytical LC techniques employed in pharmaceutical analysis consume tremendous amounts of hazardous solvents and consequently generate large amounts of waste. The monetary and ecological impact of using large amounts of solvents and waste disposal motivated the analytical community to search for alternatives to replace polluting analytical methodologies with clean ones. In this context, implementing the principles of green analytical chemistry (GAC) in analytical laboratories is highly desired. This review gives a comprehensive overview on different green LC pathways for implementing GAC principles in analytical laboratories and focuses on evaluating the greenness of LC analytical procedures. This review presents green LC approaches for eco-friendly analysis of pharmaceuticals in industrial, biological, and environmental matrices. Graphical Abstract Green pathways of liquid chromatography for more eco-friendly analysis of pharmaceuticals.

Bioactive glass 45S5 from diatom biosilica

Directory of Open Access Journals (Sweden)

Luqman A. Adams

2017-12-01

Full Text Available A major draw-back to large scale production of bioactive glasses is the high cost of the standard silica precursor, usually tetraethyl orthosilicate (TEOS. The current study describes a novel sol–gel preparation of 45S5 bioactive glass using diatom biosilica from cultured cells of the diatom, Aulacoseira granulata as substitute to TEOS. The glass formed was characterized using mechanical tester, scanning electron microscopy (SEM, energy dispersive X-ray analysis (EDX, X-ray diffraction (XRD and Fourier transform infrared (FTIR spectroscopy. Results showed that the glass possessed a compressive strength of 3.75 ± 0.18 and formed carbonated hydroxyapatite (HCA within 7 days in simulated body fluid (SBF, attributable to good surface chemistry. The performance of the glass was compared with that of those formed using TEOS. Diatom biosilica could be a potential economically friendly starting material for large scale fabrication of bioactive glasses.

Comprehensive two-dimensional gas chromatography for biogas and biomethane analysis.

Science.gov (United States)

Hilaire, F; Basset, E; Bayard, R; Gallardo, M; Thiebaut, D; Vial, J

2017-11-17

The gas industry is going to be revolutionized by being able to generate bioenergy from biomass. The production of biomethane - a green substitute of natural gas - is growing in Europe and the United-States of America. Biomethane can be injected into the gas grid or used as fuel for vehicles after compression. Due to various biomass inputs (e.g. agricultural wastes, sludges from sewage treatment plants, etc.), production processes (e.g. anaerobic digestion, municipal solid waste (MSW) landfills), seasonal effects and purification processes (e.g. gas scrubbers, pressure swing adsorption, membranes for biogas upgrading), the composition and quality of biogas and biomethane produced is difficult to assess. All previous publications dealing with biogas analysis reported that hundreds of chemicals from ten chemical families do exist in trace amounts in biogas. However, to the best of our knowledge, no study reported a detailed analysis or the implementation of comprehensive two-dimensional gas chromatography (GC×GC) for biogas matrices. This is the reason why the benefit of implementing two-dimensional gas chromatography for the characterization of biogas and biomethane samples was evaluated. In a first step, a standard mixture of 89 compounds belonging to 10 chemical families, representative of those likely to be found, was used to optimize the analytical method. A set consisting of a non-polar and a polar columns, respectively in the first and the second dimension, was used with a modulation period of six seconds. Applied to ten samples of raw biogas, treated biogas and biomethane collected on 4 industrial sites (two MSW landfills, one anaerobic digester on a wastewater treatment plant and one agricultural biogas plant), this analytical method provided a "fingerprint" of the gases composition at the molecular level in all biogas and biomethane samples. Estimated limits of detection (far below the μgNm -3 ) coupled with the resolution of GC×GC allowed the comparison

Polychlorinated biphenyls (PCB) analysis report for solid sample from 219S tank 104

International Nuclear Information System (INIS)

Ross, G.A.

1998-01-01

A sample of solids was obtained from tank 104 of 219S via a peristaltic pump equipped with a stainless steel tube and Norprenel tubing (Phthalate free). The sample obtained in a glass jar with Teflon 2 lid, was analyzed for PCBs as Aroclor mixtures. A soxhlet extraction procedure was used to extract the Aroclors from the sample. Analysis was performed using dual column confirmation gas chromatography/electron capture detection (GC/ECD). The extraction method closely follows SW-846 method 3540C and the analysis follows SW-846 method

lead glass brick

CERN Multimedia

When you look through the glass at a picture behind, the picture appears raised up because light is slowed down in the dense glass. It is this density (4.06 gcm-3) that makes lead glass attractive to physicists. The refractive index of the glass is 1.708 at 400nm (violet light), meaning that light travels in the glass at about 58% its normal speed. At CERN, the OPAL detector uses some 12000 blocks of glass like this to measure particle energies.

Coupling of In Vitro Bioassays with Planar Chromatography in Effect-Directed Analysis.

Science.gov (United States)

Weiss, Stefan C; Egetenmeyer, Nicole; Schulz, Wolfgang

Modern analytical test methods increasingly detect anthropogenic organic substances and their transformation products in water samples and in the environment. The presence of these compounds might pose a risk to the aquatic environment. To determine a possible (eco)toxicological risk, aquatic samples are tested using various bioassays, including sub-organismic assays such as the luminescent bacteria inhibition test, the acetylcholinesterase inhibition test, and the umu-test. The effect-directed analysis (EDA) combines physicochemical separation methods with biological (in vitro) tests. High-performance thin-layer chromatography (HPTLC) has proved to be particularly well suited for the separation of organic compounds and the subsequent analysis of effects by the application of the biotests directly on the surface of the HPTLC plate. The advantage of using HPTLC in comparison to high-performance liquid chromatography (HPLC) for EDA is that the solvent which is used as a mobile phase during chromatography is completely evaporated after the separation and therefore can no longer influence the applied bioassays.A prioritization during the complex identification process can be achieved when observed effects are associated with the separated zones in HPTLC. This increases the probability of identifying the substance responsible for an adverse effect from the multitude of organic trace substances in environmental samples. Furthermore, by comparing the pattern of biological effects of a separated sample, it is possible to track and assess changes in biological activity over time, over space, or in the course of a process, even without identifying the substance. HPTLC has already been coupled with various bioassays.Because HPTLC is a very flexible system, various detection techniques can be used and combined. In addition to the UV/Vis absorption and fluorescence measurements, TLC can also be coupled with a mass spectrometer (MS) for compound identification. In addition

Strengthened glass for high average power laser applications

International Nuclear Information System (INIS)

Cerqua, K.A.; Lindquist, A.; Jacobs, S.D.; Lambropoulos, J.

1987-01-01

Recent advancements in high repetition rate and high average power laser systems have put increasing demands on the development of improved solid state laser materials with high thermal loading capabilities. The authors have developed a process for strengthening a commercially available Nd doped phosphate glass utilizing an ion-exchange process. Results of thermal loading fracture tests on moderate size (160 x 15 x 8 mm) glass slabs have shown a 6-fold improvement in power loading capabilities for strengthened samples over unstrengthened slabs. Fractographic analysis of post-fracture samples has given insight into the mechanism of fracture in both unstrengthened and strengthened samples. Additional stress analysis calculations have supported these findings. In addition to processing the glass' surface during strengthening in a manner which preserves its post-treatment optical quality, the authors have developed an in-house optical fabrication technique utilizing acid polishing to minimize subsurface damage in samples prior to exchange treatment. Finally, extension of the strengthening process to alternate geometries of laser glass has produced encouraging results, which may expand the potential or strengthened glass in laser systems, making it an exciting prospect for many applications

Column Chromatography To Obtain Organic Cation Sorption Isotherms.

Science.gov (United States)

Jolin, William C; Sullivan, James; Vasudevan, Dharni; MacKay, Allison A

2016-08-02

Column chromatography was evaluated as a method to obtain organic cation sorption isotherms for environmental solids while using the peak skewness to identify the linear range of the sorption isotherm. Custom packed HPLC columns and standard batch sorption techniques were used to intercompare sorption isotherms and solid-water sorption coefficients (Kd) for four organic cations (benzylamine, 2,4-dichlorobenzylamine, phenyltrimethylammonium, oxytetracycline) with two aluminosilicate clay minerals and one soil. A comparison of Freundlich isotherm parameters revealed isotherm linearity or nonlinearity was not significantly different between column chromatography and traditional batch experiments. Importantly, skewness (a metric of eluting peak symmetry) analysis of eluting peaks can establish isotherm linearity, thereby enabling a less labor intensive means to generate the extensive data sets of linear Kd values required for the development of predictive sorption models. Our findings clearly show that column chromatography can reproduce sorption measures from conventional batch experiments with the benefit of lower labor-intensity, faster analysis times, and allow for consistent sorption measures across laboratories with distinct chromatography instrumentation.

[Analysis of pigments from Rhodotorula glutinis by Raman spectroscopy and thin layer chromatography].

Science.gov (United States)

Yuan, Yu-feng; Tao, Zhan-hua; Wang, Xue; Li, Yong-qing; Liu, Jun-xian

2012-03-01

The pigments from Rhodotorula glutinis were separated by using thin layer chromatography, and the result showed that Rhodotorula glutinis cells could synthesize at least three kinds of pigments, which were beta-carotene, torulene, and torularhodin. The Raman spectra based on the three pigments were acquired, and original spectra were preprocessed by background elimination, baseline correction, and three-point-smoothing, then the averaged spectra from different pigments were investigated, and the result indicated that Raman shift which represents C-C bond was different, and the wave number of beta-carotene demonstrated the largest deviation, finally torulene and torularhodin in Rhodotorula glutinis had more content than beta-carotene. Quantitative analysis of Raman peak height ratio revealed that peak height ratio of pigments showed little difference, which could be used as parameters for further research on living cells, providing reference content of pigments. The above results suggest that Raman spectroscopy combined with thin layer chromatography can be applied to analyze pigments from Rhodotorula glutinis, provides abundant information about pigments, and serves as an effective method to study pigments.

Design of glass-ceramic complex microstructure with using onset point of crystallization in differential thermal analysis

International Nuclear Information System (INIS)

Hwang, Seongjin; Kim, Jinho; Shin, Hyo-Soon; Kim, Jong-Hee; Kim, Hyungsun

2008-01-01

Two types of frits with different compositions were used to develop a high strength substrate in electronic packaging using a low temperature co-fired ceramic process. In order to reveal the crystallization stage during heating to approximately 900 deg. C, a glass-ceramic consisting of the two types of frits, which had been crystallized to diopside and anorthite after firing, was tested at different mixing ratios of the frits. The exothermal peaks deconvoluted by a Gauss function in the differential thermal analysis curves were used to determine the onset point of crystallization of diopside or anorthite. The onset points of crystallization were affected by the mixing ratio of the frits, and the microstructure of the glass-ceramic depended on the onset point of crystallization. It was found that when multicrystalline phases appear in the microstructure, the resulting complex microstructure could be predicted from the onset point of crystallization obtained by differential thermal analysis

Applications of liquid phase chromatographies for the analysis of streams arising at the back end of nuclear fuel cycle

International Nuclear Information System (INIS)

Deshingkar, D.S.; Yalmali, Vrunda S.; Wattal, P.K.

2000-06-01

India has opted for a closed fuel cycle comprising of reprocessing and recycling technology. The back end of such nuclear fuel cycle involves the reprocessing of spent nuclear fuels for recovery of plutonium and depleted uranium by Purex technology. Wastes arising from the reprocessing plant are classified as high, intermediate and low level wastes (HLW, ILW, LLW). HLW is mixture of over 50 elements present in different chemical forms. The accurate analyses of dissolver solution and HLW are the most challenging but essential tasks for reprocessing plant operations and also for further development of treatment methods. Inductively coupled plasma - atomic emission spectroscopy and atomic absorption spectroscopy techniques are suitable for analysis of metallic anions. Ion chromatography has proven capability to analyse number of cations or anions at ppm or even ppb level in single run. The report reviews the literature regarding the title subject. To assess the technical feasibility of ion chromatography for waste analysis, a simulated PHWR-HLW analogue was prepared. The PHWR-HLW analogue and ground water samples were analysed on DIONEX-DX 500 and Metrohm IC. Results obtained clearly demonstrated the usefulness of ion chromatography as vital analytical tool. HLW and other process or waste streams arising at the back end of nuclear fuel cycle can be analysed for alkali, alkaline earth, rare earth and transition metal cations and important anions. Use of fraction collector along with ion chromatography can enhance it's sensitivity to few Bq/ml for radioactive samples. (author)

EXTRACTION AND QUANTITATIVE ANALYSIS OF ELEMENTAL SULFUR FROM SULFIDE MINERAL SURFACES BY HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY. (R826189)

Science.gov (United States)

A simple method for the quantitative determination of elemental sulfur on oxidized sulfide minerals is described. Extraction of elemental sulfur in perchloroethylene and subsequent analysis with high-performance liquid chromatography were used to ascertain the total elemental ...

Characterization of Analytical Reference Glass-1 (ARG-1)

International Nuclear Information System (INIS)

Smith, G.L.

1993-12-01

High-level radioactive waste may be immobilized in borosilicate glass at the West Valley Demonstration Project, West Valley, New York, the Defense Waste Processing Facility (DWPF), Aiken, South Carolina, and the Hanford Waste Vitrification Project (HWVP), Richland, Washington. The vitrified waste form will be stored in stainless steel canisters before its eventual transfer to a geologic repository for long-term disposal. Waste Acceptance Product Specifications (WAPS) (DOE 1993), Section 1.1.2 requires that the waste form producers must report the measured chemical composition of the vitrified waste in their production records before disposal. Chemical analysis of glass waste forms is receiving increased attention due to qualification requirements of vitrified waste forms. The Pacific Northwest Laboratory (PNL) has been supporting the glass producers' analytical laboratories by a continuing program of multilaboratory analytical testing using interlaboratory ''round robin'' methods. At the PNL Materials Characterization Center Analytical Round Robin 4 workshop ''Analysis of Nuclear Waste Glass and Related Materials,'' January 16--17, 1990, Pleasanton, California, the meeting attendees decided that simulated nuclear waste analytical reference glasses were needed for use as analytical standards. Use of common standard analytical reference materials would allow the glass producers' analytical laboratories to calibrate procedures and instrumentation, to control laboratory performance and conduct self-appraisals, and to help qualify their various waste forms

Chromatography resin support

Science.gov (United States)

Dobos, James G.

2002-01-01

An apparatus and method of using an improved chromatography resin support is disclosed. The chromatography support platform is provided by a stainless steel hollow cylinder adapted for being inserted into a chromatography column. An exterior wall of the stainless steel cylinder defines a groove for carrying therein an "O"-ring. The upper surface of the stainless steel column is covered by a fine stainless steel mesh welded to the edges of the stainless steel cylinder. When placed upon a receiving ledge defined within a chromatography column, the "O"-ring provides a fluid tight seal with the inner edge wall of the chromatography cylinder. The stainless steel mesh supports the chromatography matrix and provides a back flushable support which is economical and simple to construct.

Ionic liquids as silica deactivating agents in gas chromatography for direct analysis of primary amines in water.

Science.gov (United States)

Krzyżaniak, Agnieszka; Weggemans, Wilko; Schuur, Boelo; de Haan, André B

2011-12-16

Analysis of primary amines in aqueous samples remains a challenging analytical issue. The preferred approach by gas chromatography is hampered by interactions of free silanol groups with the highly reactive amine groups, resulting in inconsistent measurements. Here, we report a method for direct analysis of aliphatic amines and diamines in aqueous samples by gas chromatography (GC) with silanol deactivation using ionic liquids (ILs). ILs including trihexyl(tetradecyl)phosphonium bis 2,4,4-(trimethylpentyl)phosphinate (Cyphos IL-104), 1-methyl-3-propylimidazolium bis(trifluoromethylsulfonyl)imide [pmim][Tf(2)N] and N″-ethyl-N,N,N',N'-tetramethylguanidinium tris(pentafluoroethyl)trifluorophosphate [etmg][FAP] were tested as deactivating media for the GC liner. Solutions of these ILs in methanol were injected in the system prior to the analysis of primary amines. Butane-1,4-diamine (putrescine, BDA) was used as a reference amine. The best results were obtained using the imidazolium IL [pmim][Tf(2)N]. With this deactivator, excellent reproducibility of the analysis was achieved, and the detection limit of BDA was as low as 1mM. The applicability of the method was proven for the analysis of two different primary amines (C4-C5) and pentane-1,5-diamine. Copyright © 2011 Elsevier B.V. All rights reserved.

X-ray fluorescent analysis on Indo-Pacific glass beads from Sungai Mas archaeological sites, Kedah, Malaysia

International Nuclear Information System (INIS)

Zuliskandar Ramli; Nik Hassan Shuhaimi; Nik Abdul Rahman; Abdul Latif Samian

2011-01-01

Sungai Mas was an ancient port-kingdom located on West Coast of Peninsula Malaysia in a district of Kota Kuala Muda, Kedah, Malaysia. The port-kingdom evolved as an entrepot since fifth century AD and continuously visited by international trader from India, China, Middle East and Europe until eighteenth century AD. Sungai Mas was also one of the Indo-Pacific beads making centers in Southeast Asia since sixth to thirteenth century AD and also produced pottery and brick. X-ray fluorescent analysis (XRF) on Sungai Mas Indo-Pacific beads is carried out to determine whether the glass beads originated from Arikamedu, India or locally made by community in Sungai Mas. Totally, twenty-two samples of beads and beads materials assayed by XRF were chosen. Contents of nine major elements and nine trace elements, which might be present of flux, stabilizer, colorants or opacifier were examined. The elements Si, Na, K, Ca, Fe, Al, Ti, Mn, Mg, Cu, Pb, Zr, Sr, Ba, La, U, Ni and Cr were detectable in all samples. The concentration of elements found are discussed in terms of flux, silica or lead base glass, color and/or opacity of the glass beads and glass samples. The result showed that Sungai Mas produced their own Indo-Pacific beads from sixth to thirteenth century AD. (author)

Comparison of gas chromatography/isotope ratio mass spectrometry and liquid chromatography/isotope ratio mass spectrometry for carbon stable-isotope analysis of carbohydrates.

Science.gov (United States)

Moerdijk-Poortvliet, Tanja C W; Schierbeek, Henk; Houtekamer, Marco; van Engeland, Tom; Derrien, Delphine; Stal, Lucas J; Boschker, Henricus T S

2015-07-15

We compared gas chromatography/isotope ratio mass spectrometry (GC/IRMS) and liquid chromatography/isotope ratio mass spectrometry (LC/IRMS) for the measurement of δ(13)C values in carbohydrates. Contrary to GC/IRMS, no derivatisation is needed for LC/IRMS analysis of carbohydrates. Hence, although LC/IRMS is expected to be more accurate and precise, no direct comparison has been reported. GC/IRMS with the aldonitrile penta-acetate (ANPA) derivatisation method was compared with LC/IRMS without derivatisation. A large number of glucose standards and a variety of natural samples were analysed for five neutral carbohydrates at natural abundance as well as at (13)C-enriched levels. Gas chromatography/chemical ionisation mass spectrometry (GC/CIMS) was applied to check for incomplete derivatisation of the carbohydrate, which would impair the accuracy of the GC/IRMS method. The LC/IRMS technique provided excellent precision (±0.08‰ and ±3.1‰ at natural abundance and enrichment levels, respectively) for the glucose standards and this technique proved to be superior to GC/IRMS (±0.62‰ and ±19.8‰ at natural abundance and enrichment levels, respectively). For GC/IRMS measurements the derivatisation correction and the conversion of carbohydrates into CO2 had a considerable effect on the measured δ(13)C values. However, we did not find any significant differences in the accuracy of the two techniques over the full range of natural δ(13)C abundances and (13)C-labelled glucose. The difference in the performance of GC/IRMS and LC/IRMS diminished when the δ(13)C values were measured in natural samples, because the chromatographic performance and background correction became critical factors, particularly for LC/IRMS. The derivatisation of carbohydrates for the GC/IRMS method was complete. Although both LC/IRMS and GC/IRMS are reliable techniques for compound-specific stable carbon isotope analysis of carbohydrates (provided that derivatisation is complete and the

Denaturing high-performance liquid chromatography mutation analysis in patients with reduced Protein S levels

DEFF Research Database (Denmark)

Bathum, Lise; Münster, Anna-Marie; Nybo, Mads

2008-01-01

diagnosis and risk estimation. The aim was to design a high-throughput genetic analysis based on denaturing high-performance liquid chromatography to identify sequence variations in the gene coding for Protein S. PATIENTS: In total, 55 patients referred to the Section of Thrombosis and Haemostasis, Odense......BACKGROUND: Patients with congenital Protein S deficiency have increased risk of venous thromboembolism. However, Protein S levels show large intra-individual variation and the biochemical assays have low accuracy and a high interlaboratory variability. Genetic analysis might aid in a more precise......, giving a precise diagnosis and subsequently a better risk estimation....

Contrasting the magnetic response between magnetic-glass and reentrant spin-glass

OpenAIRE

Roy, S. B.; Chattopadhyay, M. K.

2008-01-01

Magnetic-glass is a recently identified phenomenon in various classes of magnetic systems undergoing a first order magnetic phase transition. We shall highlight here a few experimentally determined characteristics of magnetic-glass and the relevant set of experiments, which will enable to distinguish a magnetic-glass unequivocally from the well known phenomena of spin-glass and reentrant spin-glass.

Rapid direct analysis to discriminate geographic origin of extra virgin olive oils by flash gas chromatography electronic nose and chemometrics.

Science.gov (United States)

Melucci, Dora; Bendini, Alessandra; Tesini, Federica; Barbieri, Sara; Zappi, Alessandro; Vichi, Stefania; Conte, Lanfranco; Gallina Toschi, Tullia

2016-08-01

At present, the geographical origin of extra virgin olive oils can be ensured by documented traceability, although chemical analysis may add information that is useful for possible confirmation. This preliminary study investigated the effectiveness of flash gas chromatography electronic nose and multivariate data analysis to perform rapid screening of commercial extra virgin olive oils characterized by a different geographical origin declared in the label. A comparison with solid phase micro extraction coupled to gas chromatography mass spectrometry was also performed. The new method is suitable to verify the geographic origin of extra virgin olive oils based on principal components analysis and discriminant analysis applied to the volatile profile of the headspace as a fingerprint. The selected variables were suitable in discriminating between "100% Italian" and "non-100% Italian" oils. Partial least squares discriminant analysis also allowed prediction of the degree of membership of unknown samples to the classes examined. Copyright © 2016. Published by Elsevier Ltd.

Analysis of human serum by liquid chromatography-mass spectrometry: improved sample preparation and data analysis.

Science.gov (United States)

Govorukhina, N I; Reijmers, T H; Nyangoma, S O; van der Zee, A G J; Jansen, R C; Bischoff, R

2006-07-07

Discovery of biomarkers is a fast developing field in proteomics research. Liquid chromatography coupled on line to mass spectrometry (LC-MS) has become a powerful method for the sensitive detection, quantification and identification of proteins and peptides in biological fluids like serum. However, the presence of highly abundant proteins often masks those of lower abundance and thus generally prevents their detection and identification in proteomics studies. To perform future comparative analyses of samples from a serum bank of cervical cancer patients in a longitudinal and cross-sectional manner, methodology based on the depletion of high-abundance proteins followed by tryptic digestion and LC-MS has been developed. Two sample preparation methods were tested in terms of their efficiency to deplete high-abundance serum proteins and how they affect the repeatability of the LC-MS data sets. The first method comprised depletion of human serum albumin (HSA) on a dye ligand chromatographic and immunoglobulin G (IgG) on an immobilized Protein A support followed by tryptic digestion, fractionation by cation-exchange chromatography, trapping on a C18 column and reversed-phase LC-MS. The second method included depletion of the six most abundant serum proteins based on multiple immunoaffinity chromatography followed by tryptic digestion, trapping on a C18 column and reversed-phase LC-MS. Repeatability of the overall procedures was evaluated in terms of retention time and peak area for a selected number of endogenous peptides showing that the second method, besides being less time consuming, gave more repeatable results (retention time: <0.1% RSD; peak area: <30% RSD). Application of an LC-MS component detection algorithm followed by principal component analysis (PCA) enabled discrimination of serum samples that were spiked with horse heart cytochrome C from non-spiked serum and the detection of a concentration trend, which correlated to the amount of spiked horse heart

Comparison of a model vapor deposited glass films to equilibrium glass films

Science.gov (United States)

Flenner, Elijah; Berthier, Ludovic; Charbonneau, Patrick; Zamponi, Francesco

Vapor deposition of particles onto a substrate held at around 85% of the glass transition temperature can create glasses with increased density, enthalpy, kinetic stability, and mechanical stability compared to an ordinary glass created by cooling. It is estimated that an ordinary glass would need to age thousands of years to reach the kinetic stability of a vapor deposited glass, and a natural question is how close to the equilibrium is the vapor deposited glass. To understand the process, algorithms akin to vapor deposition are used to create simulated glasses that have a higher kinetic stability than their annealed counterpart, although these glasses may not be well equilibrated either. Here we use novel models optimized for a swap Monte Carlo algorithm in order to create equilibrium glass films and compare their properties with those of glasses obtained from vapor deposition algorithms. This approach allows us to directly assess the non-equilibrium nature of vapor-deposited ultrastable glasses. Simons Collaboration on Cracking the Glass Problem and NSF Grant No. DMR 1608086.

Analysis of H2O in silicate glass using attenuated total reflectance (ATR) micro-FTIR spectroscopy

Science.gov (United States)

Lowenstern, Jacob B.; Pitcher, Bradley W.

2013-01-01

We present a calibration for attenuated total reflectance (ATR) micro-FTIR for analysis of H2O in hydrous glass. A Ge ATR accessory was used to measure evanescent wave absorption by H2O within hydrous rhyolite and other standards. Absorbance at 3450 cm−1 (representing total H2O or H2Ot) and 1630 cm−1 (molecular H2O or H2Om) showed high correlation with measured H2O in the glasses as determined by transmission FTIR spectroscopy and manometry. For rhyolite, wt%H2O=245(±9)×A3450-0.22(±0.03) and wt%H2Om=235(±11)×A1630-0.20(±0.03) where A3450 and A1630 represent the ATR absorption at the relevant infrared wavelengths. The calibration permits determination of volatiles in singly polished glass samples with spot size down to ~5 μm (for H2O-rich samples) and detection limits of ~0.1 wt% H2O. Basaltic, basaltic andesite and dacitic glasses of known H2O concentrations fall along a density-adjusted calibration, indicating that ATR is relatively insensitive to glass composition, at least for calc-alkaline glasses. The following equation allows quantification of H2O in silicate glasses that range in composition from basalt to rhyolite: wt%H2O=(ω×A3450/ρ)+b where ω = 550 ± 21, b = −0.19 ± 0.03, ρ = density, in g/cm3, and A3450 is the ATR absorbance at 3450 cm−1. The ATR micro-FTIR technique is less sensitive than transmission FTIR, but requires only a singly polished sample for quantitative results, thus minimizing time for sample preparation. Compared with specular reflectance, it is more sensitive and better suited for imaging of H2O variations in heterogeneous samples such as melt inclusions. One drawback is that the technique can damage fragile samples and we therefore recommend mounting of unknowns in epoxy prior to polishing. Our calibration should hold for any Ge ATR crystals with the same incident angle (31°). Use of a different crystal type or geometry would require measurement of several H2O-bearing standards to provide a crystal

Determination of dasatinib in the tablet dosage form by ultra high performance liquid chromatography, capillary zone electrophoresis, and sequential injection analysis.

Science.gov (United States)

Gonzalez, Aroa Garcia; Taraba, Lukáš; Hraníček, Jakub; Kozlík, Petr; Coufal, Pavel

2017-01-01

Dasatinib is a novel oral prescription drug proposed for treating adult patients with chronic myeloid leukemia. Three analytical methods, namely ultra high performance liquid chromatography, capillary zone electrophoresis, and sequential injection analysis, were developed, validated, and compared for determination of the drug in the tablet dosage form. The total analysis time of optimized ultra high performance liquid chromatography and capillary zone electrophoresis methods was 2.0 and 2.2 min, respectively. Direct ultraviolet detection with detection wavelength of 322 nm was employed in both cases. The optimized sequential injection analysis method was based on spectrophotometric detection of dasatinib after a simple colorimetric reaction with folin ciocalteau reagent forming a blue-colored complex with an absorbance maximum at 745 nm. The total analysis time was 2.5 min. The ultra high performance liquid chromatography method provided the lowest detection and quantitation limits and the most precise and accurate results. All three newly developed methods were demonstrated to be specific, linear, sensitive, precise, and accurate, providing results satisfactorily meeting the requirements of the pharmaceutical industry, and can be employed for the routine determination of the active pharmaceutical ingredient in the tablet dosage form. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Determination of leachable arsenic from glass ampoules

International Nuclear Information System (INIS)

Kayasth, S.R.; Swain, K.K.

2004-01-01

Appreciable amounts of different arsenic compounds are used in the manufacture of glass and glass ampoules (injection vials and bottles) used to store drugs. Exposure/intake of arsenic to human beings may result in skin ulceration, injury to mucous membranes, perforation of nasal septum, skin cancer and keratoses, especially of the palms and soles and may cause detrimental effects. Considering the toxicity of arsenic, even if traces of arsenic from such glass containers/ampoules are leached out, it can impart damage to human beings. To check the possibility of leaching of arsenic from glass ampoules, a simple methodology has been developed. Different makes and varieties of glass ampoules filled with de-ionized water were subjected to high pressure and temperature leaching for varying amount of time using autoclave to create extreme conditions for the maximum leaching out of the analyte. Subsequently, the determination of the arsenic contents in leached water using neutron activation analysis is reported in detail with observations. (author)

Diffusion structural analysis study of titania films deposited by sol-gel technique on silica glass

Czech Academy of Sciences Publication Activity Database

Balek, V.; Mitsuhashi, T.; Bountseva, I.M.; Haneda, H.; Málek, Z.; Šubrt, Jan

2003-01-01

Roč. 26, 1-3 (2003), s. 185-189 ISSN 0928-0707. [International Workshop on Glasses, Ceramics, Hybrids and Nanocomposites from Gels /11./. Abano Terme, 16.09.2001-21.09.2001] Institutional research plan: CEZ:AV0Z4032918 Keywords : titania film * diffusion structural analysis * sol-gel Subject RIV: CA - Inorganic Chemistry Impact factor: 1.546, year: 2003

Factors controlling crystallization of miserite glass-ceramic.

Science.gov (United States)

Muhammed, Fenik K; Moorehead, Robert; van Noort, Richard; Pollington, Sarah

2015-12-01

The purpose of this study was to investigate a range of variables affecting the synthesis of a miserite glass-ceramic (GC). Miserite glass was synthesized by the melt quench technique. The crystallization kinetics of the glass were determined using Differential Thermal Analysis (DTA). The glasses were ground with dry ball-milling and then sieved to different particle sizes prior to sintering. These particle sizes were submitted to heat treatment regimes in a high temperature furnace to form the GC. The crystal phases of the GC were analyzed by X-ray diffraction (XRD). Scanning electron microscopy (SEM) was used to examine the microstructure of the cerammed glass. XRD analysis confirmed that the predominant crystalline phase of the GC was miserite along with a minor crystalline phase of cristobalite only when the particle size is <20 μm and the heat treatment at 1000°C was carried out for 4h and slowly cooled at the furnace rate. For larger particle sizes and faster cooling rates, a pseudowollastonite crystalline phase was produced. Short sintering times produced either a pseudowollastonite or xonotolite crystalline phase. The current study has shown that particle size and heat treatment schedules are major factors in controlling the synthesis of miserite GC. Copyright © 2015 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

EPR investigation into the structure of boron-containing quartz glasses

International Nuclear Information System (INIS)

Amosov, A.V.; Bushmarin, D.B.; Prokhorova, T.I.; Yudin, D.M.

1975-01-01

Certain properties of boron-containing quartz glasses and the nature of occurrence of boron in the glass lattice are studied as functions of the method of alloying. The formation of three types of borate structural nodes (BO 4 , BO 3 and BO 4 -BO 3 ) in the lattice of quartz glasses is established. Alloying by boron oxide up to 3% (weight) increases the crystallization stability of quartz glasses, lowers down tsub(g) from 1220 to 950 deg C and does not affect the coefficient of thermal expansion. Low symmetry of borate structural nodes, following from the analysis of EPR spectra, confirms the literature data concerning the low symmetry of glass-forming polyhedrons in a quartz glass

Chiral-glass transition in a diluted dipolar-interaction Heisenberg system

International Nuclear Information System (INIS)

Zhang Kaicheng; Liu Guibin; Zhu Yan

2011-01-01

Recently, numerical simulations reveal that a spin-glass transition can occur in the three-dimensional diluted dipolar system. By defining the chirality of triple spins in a diluted dipolar Heisenberg spin glass, we study the chiral ordering in the system using parallel tempering algorithm and heat bath method. The finite-size scaling analysis reveals that the system undergoes a chiral-glass transition at finite temperature. - Highlights: → We define the chirality in a diluted dipolar Heisenberg system. → The system undergoes a chiral-glass transition at finite temperature. → We extract the critical exponents of the chiral-glass transition.

Diopside-Fluorapatite-Wollastonite Based Bioactive Glasses and Glass-ceramics =

Science.gov (United States)

Kansal, Ishu

Bioactive glasses and glass-ceramics are a class of biomaterials which elicit special response on their surface when in contact with biological fluids, leading to strong bonding to living tissue. This particular trait along with good sintering ability and high mechanical strength make them ideal materials for scaffold fabrication. The work presented in this thesis is directed towards understanding the composition-structure-property relationships in potentially bioactive glasses designed in CaO-MgO-P2O5-SiO2-F system, in some cases with added Na2O. The main emphasis has been on unearthing the influence of glass composition on molecular structure, sintering ability and bioactivity of phosphosilicate glasses. The parent glass compositions have been designed in the primary crystallization field of the pseudo-ternary system of diopside (CaO•MgO•2SiO2) - fluorapatite (9CaO•3P2O5•CaF2) - wollastonite (CaO•SiO2), followed by studying the impact of compositional variations on the structure-property relationships and sintering ability of these glasses. All the glasses investigated in this work have been synthesized via melt-quenching route and have been characterized for their molecular structure, sintering ability, chemical degradation and bioactivity using wide array of experimental tools and techniques. It has been shown that in all investigated glass compositions the silicate network was mainly dominated by Q2 units while phosphate in all the glasses was found to be coordinated in orthophosphate environment. The glass compositions designed in alkali-free region of diopside - fluorapatite system demonstrated excellent sintering ability and good bioactivity in order to qualify them as potential materials for scaffold fabrication while alkali-rich bioactive glasses not only hinder the densification during sintering but also induce cytotoxicity in vitro, thus, are not ideal candidates for in vitro tissue engineering. One of our bioglass compositions with low sodium

Analysis of 99mTc-labeled radiopharmaceuticals by high-performance liquid chromatography

International Nuclear Information System (INIS)

Muto, Toshio

1990-01-01

High-performance liquid chromatography (HPLC) equiped with on line radiometric and optical detectors (i.e. radio-HPLC) have been applied to the radiochemical analysis of commonly-used 99m Tc-radio pharma ceuticals with a view point to check the radiochemical purities of the compounds. Chromatographic conditions were determined by examination of the types of column, mobile phase and pH. An aqueous size-exclusion (Shim-pack Diol-300) and reversed-phase column (Zorbax-ODS) were found to be suitable for 99m Tc-HSA and the other 99m Tc-agents, respectively. The analysis of low molecular weight 99m Tc-agents (e.g. 99m Tc-DTPA, 99m Tc-DMSA, 99m Tc-pyrophosphate, 99m Tc-phytic acid, 99m Tc-MDS, 99m Tc-HMDP) were done by reversed-phaseion pairing chromatography using a optimized mobile phase consisted on a mixture of 50 mM phosphate buffer (pH 7.0) and 2 mM TBA (tetra nbutyl) ammonium hydroxide) in 30 % methanol. The mobile phases for analysis of medium molecular weight 99m Tc-HSA were consisted of a mixture of 50 mM phosphate buffer (ph 7.0) in 30 % methanol, and a mixtures of 1 % SDS (sodium dodecyl sulfonate) in Tris buffer (pH. 7.0), respectively. It was apparent from the radio-chromatograms obtained from these chromatographic conditions, that impurity of 99m TcO 4 was observed in 99m Tc-pyrophosphate, 99m Tc-phytic acid, 99m Tc-MDP, 99m Tc-HMDP, and impurities of 99m Tc-labeled species and 99m TcO 4 , were observed in 99m Tc-HIDA, 99m Tc-HIDA, 99m Tc-HSA. The radiochemical impurities of the 99m Tc-radiopharmaceuticals were ranged between 90 and 100 %. From these results, radio-HPLC has been shown to be suitable method for analysis of 99m Tc-radiopharmaceuticals, with rapidity and excellent precision. (author)

Operating Range for High Temperature Borosilicate Waste Glasses: (Simulated Hanford Enveloped)

International Nuclear Information System (INIS)

Mohammad, J.; Ramsey, W. G.; Toghiani, R. K.

2003-01-01

The following results are a part of an independent thesis study conducted at Diagnostic Instrumentation and Analysis Laboratory-Mississippi State University. A series of small-scale borosilicate glass melts from high-level waste simulant were produced with waste loadings ranging from 20% to 55% (by mass). Crushed glass was allowed to react in an aqueous environment under static conditions for 7 days. The data obtained from the chemical analysis of the leachate solutions were used to test the durability of the resulting glasses. Studies were performed to determine the qualitative effects of increasing the B2O3 content on the overall waste glass leaching behavior. Structural changes in a glass arising due to B2O3 were detected indirectly by its chemical durability, which is a strong function of composition and structure. Modeling was performed to predict glass durability quantitatively in an aqueous environment as a direct function of oxide composition