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- Author or Editor: J. Jones x
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Abstract
Traditional reaction calorimeters require highly trained operators and the use of a large sample size (10 ml to 1000 ml) which is incompatible with highly reactive substances. A new calorimeter with a 2 ml or less sample size lends itself to the determination of reactivity of materials for process safety and to the determination of safety of materials shipped in compartment tank cars. The TC-100 Titration Calorimeter meets these requirements. A cost effective instrumentation of a differential cell design provides high sensitivity heat flow measurements. Automatic liquid injection and continuous mixing provides information on the heat of reaction and its rate. A portable instrument with small sample size allows for rapid temperature equilibration and safe handling of very reactive materials.
Abstract
A radiochemical separation procedure using an inorganic exchanger, tin dioxide (TDO), for the separation of arsenic from antimony is reported here. This separation avoids the interference of 564 keV gamma-ray of122Sb in the measurement of the 559 keV gamma-ray of76As in neutron activation analysis. Environmental samples, after neutron irradiation and digestion, are taken up in 1M HCl–0.1M HF and passed through a TDO column which selectively retains arsenic. The effluent from the TDO column, after proper conditioning, is passed through an anion exchange column for quantitative retention of antimony. The procedure has been utilized for arsenic and antimony determination in NBS Orchard Leaves and NBS Albacore Tuna.
Abstract
A low cost neutron capture prompt gamma activation analysis facility has been constructed at The University of Michigan's Pheonix Memorial Laboratory. Although the neutron beam used has a fairly large epithermal component (Cd ratio 7.1), background levels are low enough to result in satisfactory measurement of over 16 different elements. For the elements of greatest sensitivity (samarium, boron, gadolinium, and cadmium) minimum detectable levels of 3.6·10−5 to 1.4·10−5 gram for a one hour measurement are possible. The fast neutrons incident to the detector were found to be minimal. Estimates of up to 3 years of continuous operation before measurable damage is expected.
Abstract
Silicon has been found to be an essential element for the growth and development of many ecomomically important plants such as sugarcane, rice, oats, and wheat. A method is described for the quantitative determination of silicon in plant samples. Measurements were made with two Ge(Li) detectors matched with a multiplexing unit to provide a single amplified signal to a computerized analyzer system. For those materials containing greater than 0.5 weight percent silicon, the reaction29Si(n, p)29Al (1273 keV) provides a direct measurement of the quantity of silicon provided the irradiation is done in a special boron nitride capsule to reduce interferences from thermal neutron reactions and a correction is made for the single escape line from28Al (1268 keV). For lesser quantities of silicon, a technique which utilizes the fast neutron reaction28Si(n, p)28Al is preferred. Corrections for the interference produced by the presence of phosphorus31P(n, α)28Al are made by determining the phosphorus content following the instrumental analysis using a unique application of neutron activation analysis, i. e., measurement of tungsten in tungstomolybdophosphoric acid produced when molybdate and tungstate ions are added to dissolved samples of the plant material containing phosphorus. Aluminum, which may also produce an interference by thermal neutron reaction27Al(n, γ)28Al, is determined directly from the original activation data after subtracting out the effect of the phosphorus. Thus, three irradiations in the pneumatic sample irradiator are necessary; one short irradiation (1 min) without thermal neutron shielding, a longer irradiation (6 min) in the boron capsule, and a final irradiation of the tungstomolybdophosphoric acid provide all data required to accurately determine silicon in plant materials. A computer program has been developed that provides rapid reduction of the data in final report format. Elements such as sodium, chlorine, calcium, manganese, potassium, and magnesium extrinsic to the analysis for silicon are also determined by this method. The method has been tested on a large number of samples and reliable results are obtained with less than 0.2 g of sample.
Abstract
The development of tritium nuclear magnetic resonance spectroscopy now makes it possible to determine the tritium distribution in virtually any organic compound at the millicurie level of radioactivity. Results of catalytic experiments show that in some cases a remarkable degree of specificity can be achieved when using procedures that are expected to produce generally labelled compounds. Conversely there are instances where specific labelling procedures are less than 100% successful.
Abstract
Our results indicate that the highest concentrations of heavy metals occurred in those plants collected near the mouth of the Saginaw River. The alga, Cladophora sp., and the flowering plant, Typha augustifolia (cat-tail), are notable for the high concentration of heavy metals that they accumulated. In addition, several other species that were sampled from small lakes in Michigan's Upper Peninsula contained higher concentrations of certain metals (Ba, Cr, Rb) than from any samples obtained from Saginaw Bay. Different organs of the same species, or of the same plant, such as cat-tail, vary widely in concentrations of the same elements. A computer-derived analysis of our data is presented, and the implications of our results as they relate to pollution by heavy metals in fresh-water lakes is discussed.
Abstract
A method for the quantitative determination of small amounts of protein samples was developed employing neutron activation analysis. Current methods of protein concentration determination are severely limited as a result of differences in the specific characteristics of each protein. Silver binding has been used as a sensitive colorimetric method to indicate the presence of protein. However, silver-protein complexes can have a variety of absorbance spectra unique to each protein, which complicate the analysis. Various amounts of specific proteins were equilibrated in an excess of silver nitrate prior to the reduction of the silver by the addition of NaBH4, HCHO, and NaOH. The protein-silver complex was rapidly separated from the unbound silver by centrifugation chromatography and the amount of bound silver was determined by INAA. The amount of silver was proportional to the amount of protein present in each sample. When the silver was not reduced prior to removal of the unbound silver by chromatography, only negligible amounts of silver remained bound to the protein. The stoichiometry of bound silver to protein on a molar basis showed relatively small differences for the proteins that were examined. This ratio was found to depend on the conditions of the binding and reduction of the silver. The results suggest that the binding of silver is not specific to any charged or polar groups on these proteins and may, therefore, provide a means of determination of the concentration of protein that has general application for all proteins.
Abstract
Three bio-fuels with or without additives and their fly ash samples were characterized using simultaneous Thermogravimetry-Differential Thermal Analysis-Fourier Transform Infrared Spectrometry-Mass Spectrometry (TG-DTA-FTIR-MS), X-ray Diffraction (XRD), X-ray Fluorescence (XRF), and Scanning Electron Microscopy-Energy Dispersive Spectrometry (SEM-EDS). The results show that the additives increase the reactivity of the bio-fuel during combustion. The additives also significantly decrease the amount of unburned carbon in the fly ash. The additives affect the compounds formed in the fly ash sample, and consequently the thermal behaviour of the fly ash. The fly ash samples are thermally stable in air up to 100C. The fly ash samples contain fine particles with irregular shape, small round particles, and large hollow spherical particles with entrapped gases.
Abstract
The conditions under which the Poisson statistical density function adequately describes the counting of a radioactive isotope are examined and found that for counting processes where λt≳1, where λ is the decay constant and t the counting period, one of the fundamental properties, namely the condition of stationarity, is violated rendering application of Poisson statistics invalid. The Ruark-Devol statistical density function, a binomial, is instead shown to be satisfactory since it is capable of describing radioactive disintegration where the only fundamental property is independence and its use is recommended in both activation analysis and medical imaging when the half-life of the isotope of interest is short compared to the period of observation. It is pointed out that no satisfactory expression incorporating the distortion produced by dead-time on the statistical density function has yet been derived but the practical implications of the adoption of the Ruark-Devol function are discussed with respect to standard deviation and precision of the measurement. It is shown how the application of the Poisson statistical density function, under conditions of tλ≳1, is not only invalid but also overestimates the standard deviation significantly.
The synthesis, compositional formula and mode of thermal decomposition of a compound for which there existed only a single literature reference [1] have been investigated in this work.
