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  • Author or Editor: H. Rook x
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Abstract  

Iodine is an element with excellent intrinsic sensitivity when determined by thermal neutron activation. However, in most real samples, the preponderance of chlorine and bromine, relative to iodine, makes the direct determination of iodine virtually impossible. Over the past 20 years, there probably have been as many publications on the separation of iodine as there have been for any other radionuclide. Upon review, however, the methods are essentially the same. After irradiation, the samples are subjected to a rapid destructive process to free the iodine from the matrix and then the iodine is separated from the other halides either by liquid-liquid extraction or by liquid ion exchange. Both of these procedures are, however, rather complex and do not effect a complete separation of the halides in one pass. In the work presented here, a simple procedure is described for the quantitative separation of iodine from chlorine. The procedure utilizes a gas phase separation on hydrated manganese dioxide with iodine collected on silvered quartz wool. The described procedure has been used for the determination of iodine in numerous new and old SRM's at the NBS.

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Abstract  

The accuracy and precision of photopeak area calculation methods has been studied by comparison of a digital method of computation with the fitting of a mathematical function to the data. In the present study, peak areas for 16 replicate photopeaks were computed both by the total peak area method any by the peak fitting method of program SAMPO. Both methods worked well with the fitting method showing somewhat smaller spread in the results.

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Abstract  

Low temperature ashing is a convenient first step in many procedures of analytical chemistry as well as a potential processing method for storing environmental samples for extended periods of time. Using activation analysis, it is shown in a number of NBS Standard Reference Materials that of some 40 elements studied, the only elements observed to be lost were osmium, mercury and halogens along with carbon. No contamination during the ashing process was detected.

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Abstract  

Potentially toxic metals in the food chain that can lead to deleterious effects on human health have been well documented. Because of the toxicity of some metals, levels of 1 ppm or less must be routinely monitored in foods to ensure human safety. To ensure the accuracy of measurement, NBS in a cooperative interagency agreement with the Food and Drug Administration is involved in developing and certifying selected elements in food grain as a part of the Standard Reference Material program. Both instrumental and radiochemical neutron activation analysis were used to analyze two food grain standard reference materials (Rice and Wheat Flours) for trace element certification.

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Abstract  

The application of high yield mass separators to problems in activation analysis is discussed. The identification of separation parameters including separator yields, memory, resolution and overlap, and sputtering are considered. The use of the mass separator in determining lead by photon activation analysis is described.

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Abstract  

Since the late 1990’s, research has been reported where intercalated, expanded, and/or exfoliated graphite nanoflakes could also be used as reinforcements in polymer systems. The key point to utilizing graphite as a platelet nanoreinforcement is in the ability to exfoliate graphite using Graphite Intercalated Compounds (GICs). Natural graphite is still abundant and its cost is quite low compared to the other nano–size carbon materials, the cost of producing graphite nanoplatelets is expected to be ~$5/lb. This is significantly less expensive than single wall nanotubes (SWNT) (>$45000/lb) or vapor grown carbon fiber (VGCF) ($40–50/lb), yet the mechanical, electrical, and thermal properties of crystalline graphite flakes are comparable to those of SWNT and VGCF. The use of exfoliated graphite flakes (xGnP) opens up many new applications where electromagnetic shielding, high thermal conductivity, gas barrier resistance or low flammability are required. A special thermal treatment was developed to exfoliate graphite flakes for the production of nylon and high density polypropylene nanocomposites. X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM) were used to assess the degree of exfoliation of the graphite platelets and the morphology of the nanocomposites. The thermal conductivity of these composites was investigated by three different methods, namely, by DSC, modified hot wire, and halogen flash lamp methods. The addition of small amounts of exfoliated graphite flakes showed a marked improvement in thermal and electrical conductivity of the composites.

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