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  • Author or Editor: Min Wei x
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Planar electrochromatography in the reversed-phase mode has been performed in a commercially available development chamber, which requires only small modification for this purpose. This report illustrates that good separation quality and good reproducibility can both be obtained by use of this apparatus. Only short migration distances — less than 4.0 cm — were obtained under the conditions used.

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Abstract

Methyl ethyl ketone peroxide (MEKPO), which has highly reactive and exothermically unstable characteristics, has been extensively employed in the chemical industries. It has also caused many thermal explosions and runaway reaction accidents in manufacturing processes during the last three decades in Taiwan, Japan, Korea, and China. The goal of this study was to simulate thermal upset by MEKPO for an emergency response. Vent sizing package 2 (VSP2) was used to determine the thermokinetics of 20 mass% MEKPO. Data of thermokinetics and hazard behaviors were employed to simulate thermal explosion in three types of vessel containing 20 mass% MEKPO under various scenarios at the same volume. To compare and appraise the difference of important parameters, such as maximum temperature (T max), maximum pressure (P max), etc. This was necessary and useful for investigating the emergency response procedure associated with industrial applications.

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A conjugate of 6-hydrazinopyridine-3-carboxylic acid (HYNIC) with aminomethylenediphosphonic acid (AMDP) was synthesized through a multiple-step reaction. HYNIC–AMDP could be labeled easily and efficiently with 99mTc using N-(2-hydroxy-1,1-bis(hydroxymethyl)ethyl)glycine (tricine) as coligand to form the 99mTc–HYNIC–AMDP complex in high yield (> 95%). Its partition coefficient indicated that it was a good hydrophilic complex. The biodistribution studies of 99mTc–HYNIC–AMDP in normal ICR mice showed that this complex had high bone uptake and low or negligible accumulation in non-target organs. As compared with 99mTc–MDP, 99mTc–HYNIC–AMDP had a higher bone uptake and the ratios of bone/blood and bone/muscle at early time after injection, suggesting that it could be potentially useful for bone imaging at an earlier time after injection according to further investigations of the biological behavior of this complex.

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With two active O–O peroxide groups, 1,1-bis(tert-butylperoxy)cyclohexane (BTBPC) has a certain degree of thermal instability. It is usually used as an initiator in chemical processes, and therefore reckless operation may result in serious thermal accidents. This study focused on the runaway reactions of BTBPC alone and mixed with various concentrations of nitric acid (1, 2, 4, and 8 N). The essential thermokinetic parameters, such as exothermic onset temperature (T o), activation energy (E a), frequency factor (A), time to maximum rate under adiabatic condition (TMRad) and time to conversion limit (TCL), were evaluated by differential scanning calorimetry at the heating rate of 4 °C min−1, and a kinetics-based curve fitting method was used to assess the thermokinetic parameters. All the results indicated that BTBPC mixed with one more than 4 N nitric acid dramatically increased the degree of thermal hazard in the exothermic peak and became more dangerous. However, it was relatively safe for BTBPC mixed with less than 1 N nitric acid under 34.5 °C.

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The decomposition of organic peroxides by their relatively weak oxygen linkage and hydroperoxide radical in the presence of reaction solution is one of the thermal hazards for triggering a runaway reaction. Runaway incidents may occur in oxidation reactors, vacuum condensation reactors, tank lorries, or storage tanks. In NFPA 432 organic peroxides in NFPA 432 are classified as flammable. The exothermic behaviors of solid organic peroxides, dicumene peroxide, benzoyl peroxide, and lauroyl peroxide, were determined by differential scanning calorimetry (DSC), and vent sizing package 2 (VSP2). Relevant data detected by DSC provided thermal stability information, such as exothermic onset temperature (T 0), maximum heat-releasing peak (T max), and heat of decomposition (ΔH d). VSP2 was used to perform the bench scale situation for pushing the expected or unexpected reaction to undergo runaway reaction. Onset temperature, maximum pressure, self-heating rate ((dT dt −1)max), and pressure-release rate ((dP dt −1)max) were therefore obtained and explained. These results are essentially crucial in process design for an inherently safer approach.

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In this work, a simple group separation scheme based on extraction for NAA determination of trace of As, Cd, Hg, Cu and Zn in biological materials is described. For this purpose, zinc-diethyldithiocarbamate, Zn(DDC)2, and methyl isobutyl ketone-iodide have been chosen as reagents. The elements can be extracted successively and quantitatively from strong mineral acids without adjusting pH of the solution, and separated into two groups suitable for gamma-ray spectrometry. Samples of 100–200 mg dry weight were double-sealed into polyethylene bags and irradiated in a swimming pool reactor with a thermal neutron flux of 1013n·cm–2·s–1 for 44 hours. After a cooling period of 1–3 days, the samples were digested with microgram quantities of carrier in concentrated nitric acid and sulfuric acid at 150°C for 3.5 hours in a teflon bomb, then extracted as described above. The reliability of the analytical method was checked using reference materials Horse Kidney IAEA H-8, Human Hair NIES-5 and Tomato Leaves NBS-1573. Most of the results obtained for reference materials agreed with the certified values12. Chinese autopsy samples of hair and liver were presented.

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Planar electrochromatography (PEC) is a mode of planar chromatography in which the mobile phase is driven by electroosmotic flow. The variables that affect the performance of PEC with an aqueous mobile phase on a bonded octadecylsilyl layer are discussed. These include the magnitude of the applied electric field, the concentration of the buffer salt, the pH of the mobile phase, and the concentration of acetonitrile used as the organic modifier. The effect of changing each of these variables is illustrated by model separations of a mixture of four compounds of diverse structure.

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When above certain temperature limits, lauroyl peroxide is an unstable material. If the thermal source cannot be properly governed during any stage in the preparation, manufacturing process, storage or transport, runaway reactions may inevitably be induced immediately. In this study, the influence of runaway reactions on its basic thermal characteristic was assessed by evaluating thermokinetic parameters, such as activation energy (E a) and frequency factor (A) by thermal activity monitor III (TAM III). This was achieved under five isothermal conditions of 50, 60, 70, 80, and 90 °C. Vent sizing package 2 (VSP2) was employed to determine the maximum pressure (P max), maximum temperature (T max ), maximum self-heating rate ((dT dt −1)max), maximum pressure rise rate ((dP dt −1)max), and isothermal time to maximum rate ((TMR)iso) under the worst case. Results of this study will be provided to relevant plants for adopting best practices in emergency response or accident control.

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In this paper, 3-amino-1-hydroxypropylidene-1,1-bisphosphonate(APB), a amidobisphophonate was synthesized and labeled with the α-emitter 211At by an indirect method using N-succinimidyl 5-(tributylstannyl)-3-pyridinecarboxylate (SPC) as a bi-functional linker, and the conjugated amidobisphophonate (211At-SAPC-APB) was preliminarily evaluated in vitro and in vivo by comparison with free astatide (211At) and 99mTc-MDP. 3-amino-1-hydroxypropylidene-1,1-bisphosphonate(APB) was prepared using β-alanine as the starting material. With SPC bi-functional linker, APB was conjugated with 211At in a labeling yield of 80–90% with radiochemical purity of more than 99%. The conjugated amidobisphophonate (211At-SAPC-APB) exhibited considerable stability in vitro, in that the radiochemical purity of 211At-SAPC-APB was still more than 98% in 0.1 mol/L PBS (pH 7.6) or in fetal calf serum, even stayed for 24 h at room temperature (RT). Biodistribution of 211At-SAPC-APB was investigated in NIH strain mice by I.V injection. The results showed that 211At-SAPC-APB could rapidly locate in shank, with the maximum uptake of 23.70 ± 2.29% I.D/g at 6 h, earlier than that of 99mTc-MDP at 12 h, and stayed in the bone for long time. Moreover, 211At-SAPC-APB uptake in some key organs or tissues, especially in thyriod, stomach, lung and spleen, was much less than that of free astatide (211At), implying that 211At-SAPC-APB was constantly stable in vivo as well as in vitro. These results indicated that 211At-SAPC-APB will be a suitable candidate for the targeted radiotherapy of bone metastases and should be further investigated.

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Abstract  

With 2,3,5,6-tetrafluorophenyl 3-(nodo-carboranyl) propionate (TCP) as a new potential bi-functional linker, bovine serum albumin (BSA) was conjugated with 211At, and the conjugated model protein (211At-TCP-BSA) was preliminarily evaluated in vitro and in vivo by comparison with 211At-SAB-BSA and 211At-SAPC-BSA, which conjugated with 211At via aryl derivatives ATE (N-succinimidyl-3-(tri-n-butylstannyl) benzoate) or SPC (N-succinimidyl 5-(tributylstannyl)-3-pyridinecarboxylate). The radiolabeled intermediate 211At-TCP was coupled to BSA in yields ranging from 35 to 45% with radiochemical purity of more than 98%. The conjugated 211At-TCP-BSA exhibited considerable stability in vitro in 0.1 mol/L PBS (pH 7.6) at room temperature (RT), similar to 211At-SAPC-BSA and 211At-SAB-BSA. Biodistribution of the 211At conjugated protein was investigated in NIH strain mice by I.V injection. The results showed that 211At-TCP-BSA was constantly stable in vivo as well as in vitro, but more stable than 211At-SAPC-BSA and 211At-SAB-BSA. These results implied that radioastatinated carboranes based on B–At bonds are higher stability than radioastatinated aryl derivatives based on C–At to in vivo deastatination. In other word, TCP should be a promising bi-functional linker for 211At conjugation of proteins or antibodies.

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