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Organically templated thorium compounds were synthesized for the first time under hydrothermal conditions; the piperazine containing compound consists of 2-D layers, while the 2-methylpiperazine phase contains unprecedented 1-D chains of face-sharing ThF9 polyhedra.
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Two hundred seventy-three men exposed to thorium and other rare earths between 1940 and 1973 at a plant which refined monazite sand were studied at Argonne National Laboratory from 1976 to 1980. In vivo measurements of body burden were made by counting gamma rays emitted by daughter products of retained thorium and by measuring exhaled thoron. Health status was ascertained through questionnaire, physical examination, and clinical laboratory tests. Measured body burden was found to be higher in those with a history of longer exposure. All parameters of the complete blood count were examined for evidence of an effect due to thorium. Comparisons of high and low body burden groups showed that only age and cigarette smoking had an effect on complete blood count parameters.
Unlike the parent (C3H5)4Th that decomposes at 0 degrees C, homoleptic tetra(allyl)thorium complexes [(SiMe3)nC3H5-n]4Th (n = 1, 2) have been prepared from ThBr4(thf)4 and K[(SiMe3)nC3H5-n] that are stable up to 90 degrees C (n = 1) or 124 degrees C (n = 2). The molecules, which are fluxional on the NMR time scale, contain the first structurally authenticated Th-allyl bonds. The trimethylsilyl groups cause relatively little perturbation in the core metal-allyl geometry but markedly increase the kinetic stability of the compounds.
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The efficacy of CaDTPA and ZnDTPA, the chelating agents of choice for several actinide elements, have been evaluated after the deposition of thorium in the rat lung in widely different amounts. The results showed that: 1. When the initial mass concentration of thorium simulated human exposure to four times the annual limits on intake for 232Th, the prompt (300 or 1000 mumol kg-1 body weight at 0.02 d) or repeated (30 or 300 mumol kg-1 body weight at 0.02, 0.25, 1,2,3 d) administration of CaDTPA were at best only moderately successful for enhancing the elimination of thorium. By 7 d after exposure, the body contents of thorium were, respectively, about 74%, 65%, 90% and 74% of those present in untreated animals. 2. When the mass concentration simulated 1.7 x 10(-3) times the annual limits on intake for 232Th, the efficacy of treatment was not increased appreciably despite the substantial reduction in mass. After the repeated administration of CaDTPA at doses of 30 and 300 mumol kg-1 using the protocol above, the body contents of thorium by 7 d were, respectively, 69% and 51% of those in untreated animals. 3. Under comparable conditions, the efficacy of ZnDTPA was less than CaDTPA. The results suggest that more effective chelating agents are needed for the treatment of workers exposed to water soluble thorium compounds.
The translocation of 234Th from a simulated wound site and the efficacy of DTPA administration, as a function of the thorium compound injected as well as the DTPA treatment schedule, have been investigated in rats. Much more 234Th injected as citrate was translocated from the injection site than after administration as nitrate, whereas the distribution pattern of 234Th translocated to the various tissues was nearly identical for both 234Th compounds. Combined local and systematic treatment with DTPA was equally or more effective than each of the treatments alone in reducing the retention of 234Th at the injection site and in the organs.
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Thorium and iodine memory effects have been characterized experimentally for inductively-coupled plasma mass spectrometry by adding ammonia gas directly to the spray chamber and nebulizing aqueous ammonia sample solutions to assess analyte memory retention sites. Thorium memory effect originates from the tendency of an unidentified thorium compound to volatilize from the spray-chamber walls, and not from Th compound adsorption to nebulizer tubing. The mass spectrometer skimmer and sampler cones, ion optics, quadrupole, and other components are not responsible for the memory effect. Unlike that of thorium the iodine memory effect originates from adsorption of iodine compounds on nebulizer tubing surfaces and from volatilization of HI and I2 from the spray-chamber walls. Addition of ammonia sample solutions or ammonia gas directly to the spray chamber eliminated the Th and I memory effects in practical analyses, and blank levels were achieved after 2 min wash-outs. Quantitative recoveries were obtained for Th and I in reference materials.
We have shown that a scanning transmission electron microscope with a high brightness field emission source is capable of obtaining better than 3 A resolution using 30 to 40 keV electrons. Elastic dark field images of single atoms of uranium and mercury are shown which demonstrate this fact as determined by a modified Rayleigh criterion. Point-to-point micrograph resolution between 2.5 and 3.0 A is found in dark field images of micro-crystallites of uranium and thorium compounds. Furthermore, adequate contrast is available to observe single atoms as light as silver.
Ultrasonic irradiation (22 kHz, Ar atmosphere) of Th(IV) beta-diketonates Th(HFAA)4 and Th(DBM)4, where HFAA and DBM are hexafluoroacetylacetone and dibenzoylmethane respectively, causes them to decompose in hexadecane solutions, forming solid thorium compounds. The first-order rate constants for Th(IV) beta-diketonate degradation were found to be (9.3 +/- 0.8) x 10(-3) for Th(HFAA)4 and (3.8 +/- 0.4) x 10(-3) min-1 for Th(DBM)4, (T = 92 degrees C, I = 3 W cm-2). The rate of the sonochemical reaction increased with the rising beta-diketonate volatility and decreased with the rising hydrocarbon solvent vapor pressure. Solid sonication products consisted of a mixture of thorium carbide ThC2 and Th(IV) beta-diketonate partial degradation products. The average ThC2 particle size was estimated to be about 2 nm. ThC2 formation was attributed to the high-temperature reaction occurring within the cavitating bubble. The thorium beta-diketonate partial degradation products formed in the liquid reaction zones surrounding the cavitating bubbles.
Analytical microscopy was used to study the distribution and chemical composition of thorium deposits in bone marrow and liver after injection of thorium dioxide and thorium nitrate. Thorotrast (thorium dioxide) was identified as being localized in bone marrow macrophages of a patient who had undergone cerebral arteriography forty two years ago. Large thorotrast deposits were also present in liver cells. We show that non-colloidal thorium (thorium nitrate) injected in rats concentrates in a non soluble form in bone marrow macrophages, hepatocytes and Kupffer cells. These deposits of thorium associated with phosphorus can be explained by the formation of thorium phosphate in lysosomes and we demonstrate that they remain in tissue for a long time. Microanalysis was performed with ion microscopy, and electron probe microanalysis by X ray spectrometry, which can identify and localize thorium and associated elements at cellular or intracellular level.
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