Liposomes in analyses

The use of liposomes as analytical and bioanalytical reagents has been shown to be successful of in a variety of different applications that will be reviewed here. Due to their high surface area, large internal volume, and ability to conjugate bilayer lipids with a variety of biorecognition elements liposomes have been used in homogenous and heterogeneous assays, providing signal amplification both as intact or lysed vesicles. This review covers the discussion of their application in recent liposome-based immunoassay publications and includes the growing number of other non-immunoassay applications as an evidence of their immense versatility. In this article, a general background about liposomes is given first that extends past the use of liposomes as analytical tools. The main discussion is then divided by the manner in which liposomes are utilized as signaling reagents for the assays. Where available, the detection limits for common analytes that have been assayed using multiple liposome-based detection systems are presented. The advantages of using liposomes in terms of sensitivity versus other techniques are also discussed.     

Vibrational analyses of silacyclopentanes

The complete infrared and Raman spectra of 1,1-difluoro-1-silacyclopentane and 1,1-dichloro-1-silacyclopentane have been recorded and analyzed. Furthermore, a number of the vibrational frequencies of the silacyclopentane and silacyclopentane-1, 1-d₂ molecules have been reassigned.A normal coordinate calculation for each of these molecules was carried out and this demonstrated the validity of the assignments. Considerable mixing of the modes was found especially where ring vibrations and SiX₂ motions were involved.     

Thermal analyses of aerosols

Thermal analysis as an analytical tool has been applied to the study of suspended liquid and solid matter in air. The aerosol is heated in a glass pipe, and the light scattering coefficient is used for thein situ detection of aerosol. Results of thermal analysis of the Los Angeles smog, and of St. Louis aerosol on dry and humid days, are presented, all indicating distinctly different thermo-nephelograms. On polluted days in St. Louis, over 50% of the light scattering coefficient is lost at about 100, which indicates the presence of H₂SO₄.

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Zusammenfassung Die Thermoanalyse wurde als analytische Methode zur Untersuchung von in Luft suspendierten flüssigen und festen Substanzen eingesetzt. Das Aerosol wird in einem Glasrohr beheizt und Lichtstreuungskoeffizient zumin situ Nachweis des Aerosols verwendet. Die Ergebnisse der Thermoanalyse von Smog aus Los Angeles und von Aerosol aus St. Louis an trockenen und feuchten Tagen werden bekanntgegeben; diese zeigen deutlich verschiedene Thermonephelogramme. An Tagen bei besonders starker Verschmutzung in St. Louis, gehen mehr als 50% des Lichtstreuungskoeffizienten bei etwa 100 verloren, was auf Gegenwart von H₂SO₄ zurückzuführen ist.

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Résumé Application de l'analyse thermique comme moyen d'analyse des matériaux liquides et solides en suspension dans l'air. L'aérosol est chauffé dans un tube de verre et le coefficient de diffusion de la lumière est utilisé pour analyserin situ l'aérosol. Les résultats de l'analyse du brouillard de Los Angeles et de l'aérosol de St. Louis par temps sec et humide sont présentés, indiquant tous des néphélogrammes thermiques différents. Les cas de pollution à St. Louis se traduisent par une déperdition du coefficient de diffusion de la lumière de plus de 50% à 100 environ, ce qui indique la présence de H₂SO₄.

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This research was supported by the U.S. Environmental Protection Agency, National Environmental Research Center, Atmospheric Aerosol Research Section, Research Triangle Park, N.C.     

Gas hydrate single-crystal structure analyses

The first single-crystal diffraction studies on methane, propane, methane/propane, and adamantane gas hydrates SI, SII, and SH have been performed. To circumvent the problem of very slow crystal growth, a novel technique of in situ cocrystallization of gases and liquids resulting in oligocrystalline material in a capillary has been developed. With special data treatment, termed oligo diffractometry, structural data of the gas hydrates of methane, acetylene, propane, a propane/ethanol/methane-mixture and an adamantane/methane-mixture were obtained. Cell parameters are in accord with reported values. Host network and guest are subject to extensive disorder, reducing the reliability of structural information. It was found that most cages are fully occupied by a guest molecule with the exception of the dodecahedral cage in the acetylene hydrate which is only filled to 60%. For adamantane in the icosahedral cage a disordered model is proposed.     

Molecular spectroscopic analyses of gelatin

The molecular structure of gelatin was studied using Fourier transform infrared spectroscopy FTIR. The spectrum is subjected to deconvolution in order to elucidate the constituents of the molecular structure. B3LYP/6-31g** was used to study 13 amino acids then the scaled spectrum was compared to those of protein in order to describe the contribution of each amino acid into protein structure. A special interest was paid to the NH and C=O region. The reactivity of each amino acid was studied in terms of some important physical parameters like total dipole moment and HOMO/LUMO which describe the interaction of amino acid with their surrounding molecules. Results indicated that B3LYP/6-31g** model is a suitable and precise method for studying molecular structure of protein.     

Thermal analyses of coordination compounds

The compounds [PdCl₂L₂] and [PdL₄] (L=PPh₃, AsPh₃, SbP₃) were studied by thermogra-vimetric and differential thermal analyses in air. The residues of thermal decomposition consist of metallic palladium, except in the case of the complexes containing SbPh₃, when the residues are palladium and antimony mixtures in appropriate proportions with respect to the stoichiometry of the related complexes.     

Vibrational analyses employing cartesian coordinates

Geometry-optimised ab initio (STO-3G minimal basis set) calculations have been carried out for S-trans and orthogonal forms of 1,3-butadiene. The central C-C bond is shorter (1.482 Å) in the S-trans form than the orthogonal form (1.504 Å). Calculations on the orthogonal form indicate that the additional bond length decrease destabilizes the σ bond. the stabilization of the S-trans form being associated with conjugative (or π delocalization) effects.     

Ultrahigh sensitivity uranium analyses using fission track counting: Further analyses of semiconductor packaging materials

Neutron activation analysis with fission track counting was applied to a study of a variety of ceramic and plastic semiconductor packaging materials. By using a high purity synthetic fused silic as a detector, the method has a lower limit for uranium of 0.02 ppb. The highly sensitive, accurate technique permitted study of individual, highly contaminated glass fibers in molded plastics and also studies of bulk ceramic and plastic materials.     

XAFS analyses of molten metal fluorides

X-ray absorption fine structure studies of molten metal fluorides containing the materials related to nuclear engineering are intensively summarized. By using XAFS spectra data of divalent and trivalent cation metal fluorides in molten state which have been collected by authors’ group for a few years, local structure have been extracted and discussed systematically in conjunction with other spectroscopic studies and numerical calculations. In molten divalent fluorides, tetrahedral coordination of fluorides around a cation is predominant. In the case of pure molten trivalent fluorides, structure with more than 6-coordination has been suggested in some cases, but octahedral coordination structure is much stabilized at heavier rare earth metal fluorides. By mixing with alkali metal fluorides, it is a general trend that inter-ionic distances keep constant, but coordination number of fluorides decreases. In experimental chapter, all the details of sample preparation, furnace installation, X-ray optics setups and data analyses procedures are explained. Finally, future expectations of XAFS technique are also suggested.     

Ion beam analyses of carbon nanotubes

The utility of ion beam analysis (IBA) techniques to quantitatively determine impurities in carbon nanotubes (CNTs) over a wide range of atomic numbers is demonstrated. Such techniques have not previously been used to monitor impurities and their effects in this unique material. Despite the difficulty in mounting the samples (which generally are formed into a powdery aggregate rather in a thin film), it is shown that reliable and accurate measurements of impurity concentrations can be achieved. Particle-induced X-ray emission (PIXE) and elastic recoil detection (ERD) analyses were used to characterize both metallic and very light (e.g., hydrogen) impurities in CNTs. This paper reports the first direct measurement of hydrogen in CNTs using an IBA technique. This is significant because CNTs are being actively investigated for hydrogen storage technology for energy applications.     

Carbohydrate analyses with high-performance anion-exchange chromatography

High-performance anion-exchange chromatography (HPAEC), in tandem with pulsed amperometric detector (PAD) is a powerful tool for carbohydrate analysis. It requires no pre- or postcolumn derivatization, and yet offers superb resolution and sensitiviy. In its basic mode, alcoxide anions from the hydroxyl groups of carbohydrates as well as other anionic substituents are utilized. In addition to the number of hydroxyl groups, separation can be based on anomers, positional isomers, as well as degree of polymerization.     

Thermal analyses of Ohio bituminous coals

A suite of twenty-one bituminous coal samples from Ohio were analyzed by differential scanning calorimetry (DSC) and non-isothermal thermogravimetry (TG) techniques. Three regions of endothermic activity may be distinguished in the DSC scans in an inert atmosphere. The first peak (25–150°C) corresponds to loss of moisture from the coal, a second, very broad endotherm peaking in the range 400–500°C corresponds to devolatilization of the organic matter and a partially resolved endotherm at temperatures above 550°C probably corresponds to cracking and coking processes subsequent to the pyrolysis step. Evidence obtained from experiments with sealed pans suggest an autocatalytic effect exerted by the pyrolysis products. The use of the DSC technique to quantify the volatile matter content of coal seems less reliable than the proximate analyses obtained from non-isothermal TG in inert and O₂ atmospheres. Good agreement with ASTM values is observed by the latter method for a range of volatile matter and ash content.     

Accuracy in analyses of biological materials

Summary The work of the Community Bureau of Reference is outlined, special emphasis being laid on the problem of accuracy. Examples are described for trace elements in milk, Pb and Cd in blood, Ca in serum, cortisol in serum and aflatoxin in milk.     

On-line slurry analyses by californium-252

In chemical processing technology on-line activation methods gain an increasing importance for process monitoring and control. In the paper presented a method is described according to which the different fluorspar contents at various strategic points of a flotation plant are to be determined through neutron activation by 100 μg²⁵² californium. For that purpose, a continuous analytical system for on-stream process control of slurries was designed and constructed. This SUSAC compact facility allows continuous application of the method on an industrial scale.     

Quantitative analyses of impurities in ZnO

Problems on the quantitative analyses of impurities in secondary ion mass spectrometry (SIMS) were revealed by analysing standard samples. One problem is the interference confirmed when ²⁷Al¹⁶O, ⁶³Cu and ⁶⁷Zn¹⁶O negative ions were measured, which can be avoided by measuring a high‐resolution mass spectrum. Another problem is that light elements such as hydrogen can be measured accurately only after using a cooling system to reduce the background intensity. These remedies were applied in the quantitative analysis of single‐crystal ZnO grown by hydrothermal and vapour transport techniques. Copyright © 2004 John Wiley & Sons, Ltd.     

Radiochemical analyses using EmporeTM Disk Technology

Two studies expanding the customary use of 3M Empore^TM Rad Disks have been conducted. In the first study,²²⁶Ra and²²⁸Ra were determined simultaneously by an improved method that used a single gamma-spectroscopy analysis. In the second study, various tracer materials and procedures were used to correct for yield losses in the determination of⁹⁰Sr and⁹⁹Tc in synthetic samples that contained significant interferences.