Activation of Zero-Valent Magnesium using Acetic Acid for the Degradation of Triacetone Triperoxide in Ethanol
Abstract
Triacetone triperoxide (TATP), a cyclic peroxide, is an explosive frequently used by terrorists and amateur chemists due to the ease of synthesis and the availability of reagents. A degradation method for degrading TATP in ethanol (EtOH) was proposed using an activated, zero-valent magnesium (ZVMg) system. Different acids were tested to determine their effectiveness in activating Mg for the degradation of TATP, and short chain carboxylic acids, particularly acetic acid, were observed to have the greatest effect on the TATP degradation rate. Other ZVMg systems were also tested including ZVMg mechanically alloyed
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The TATP/EtOH solution was exposed to 0.25 g of Mg, Mg/Pd, or Mg/C. For statistical analysis, all experiments were performed in duplicate. Depending on the individual kinetic study, the different quantities of acid were added immediately after the addition of the TATP solution to the metal. Any unreacted TATP was extracted using toluene, and the reaction mixture was filtered using a nylon Puradisc® syringe filter (2 μm pore size) to remove the reacted metal. Water was added to the extracted solution to remove the EtOH from the toluene layer, and the sample was shaken for 2 min then centrifuged at 1200 rpm for 4 min. The organic layer was then removed for analysis using …show more content…
1, ZVMg in EtOH (with no acid) did not readily degrade TATP during the 4.5 hour reaction time period. Due the inactivity of ZVMg in the degradation of TATP in EtOH, attempts were made to activate the ZVMg particles in EtOH. Mg/Pd had been used to degrade TATP in a water/methanol solvent [12], thus the mechanically alloyed Mg/Pd was also tested in EtOH solvent. Similar to the ZVMg system, TATP degradation was not achieved using the mechanically alloyed Mg/Pd in EtOH (Fig. 2). Additional methods were then attempted to activate the ZVMg and Mg/Pd systems for the degradation of TATP in
Some possible errors raised during the synthesis and spectrometric analysis of TPCP include the insufficient mixing of the hexane and TPCP, in which will result in the low absorbance of the compound. Additionally, the low yield is contributed from the loss of product during filtration.
In a small reaction tube, the tetraphenylcyclopentadienone (0.110 g, 0.28 mmol) was added into the dimethyl acetylene dicarboxylate (0.1 mL) and nitrobenzene (1 mL) along with a boiling stick. The color of the mixed solution was purple. The solution was then heated to reflux until it turned into a tan color. After the color change has occurred, ethanol (3 mL) was stirred into the small reaction tube. After that, the small reaction tube was placed in an ice bath until the solid was formed at the bottom of the tube. Then, the solution with the precipitate was filtered through vacuum filtration and washed with ethanol. The precipitate then was dried and weighed. The final product was dimethyl tertraphenylpthalate (0.086 g, 0.172mmol, 61.42%).
The goal of this two week lab was to examine the stereochemistry of the oxidation-reduction interconversion of 4-tert-butylcyclohexanol and 4-tert-butylcyclohexanone. The purpose of first week was to explore the oxidation of an alcohol to a ketone and see how the reduction of the ketone will affect the stereoselectivity. The purpose of first week is to oxidize the alcohol, 4-tert-butylcyclohexanol, to ketone just so that it can be reduced back into the alcohol to see how OH will react. The purpose of second week was to reduce 4-tert-butylcyclohexanol from first week and determine the effect of the product's diastereoselectivity by performing reduction procedures using sodium borohydride The chemicals for this lab are sodium hypochlorite, 4-tert-butylcyclohexanone
...e 3. Both letters A and B within the structure of trans-9-(2-phenylethenyl) anthracene, that make up the alkene, have a chemical shift between 5-6 ppm and both produce doublets because it has 1 adjacent hydrogen and according to the N + 1 rule that states the number of hydrogens in the adjacent carbon plus 1 provides the splitting pattern and the number of peaks in the split signal, which in this case is a doublet.1 Letters C and D that consist of the aromatic rings, both are multiplets, and have a chemical shift between 7-8 ppm. 1H NMR could be used to differentiate between cis and trans isomers of the product due to J-coupling. When this occurs, trans coupling will be between 11 and 19 Hz and cis coupling will be between 5 and 14 Hz, showing that cis has a slightly lowered coupling constant than trans, and therefore have their respective positions in a product. 2
This process is then repeated. In the second trial, the Mg ribbon did not completely dissolve and the results were thrown out. The third trial (referred to as the second in the following analysis due to the exclusion of the previous one) was successful, and measurements can be seen below. We then moved onto the second reaction using magnesium oxide and hydrochloric acid in the fume hood. We measured 200.1 mL of HCl and placed it in the calorimeter, and an initial temperature reading was taken.
The purpose of the experiment is to study the rate of reaction through varying of concentrations of a catalyst or temperatures with a constant pH, and through the data obtained the rate law, constants, and activation energies can be experimentally determined. The rate law determines how the speed of a reaction occurs thus allowing the study of the overall mechanism formation in reactions. In the general form of the rate law it is A + B C or r=k[A]x[B]y. The rate of reaction can be affected by the concentration such as A and B in the previous equation, order of reactions, and the rate constant with each species in an overall chemical reaction. As a result, the rate law must be determined experimentally. In general, in a multi-step reac...
9. When all magnesium has reacted, remove the lid and heat strongly for 5 minutes
Hydrogen peroxide is a liquid which contains hydrogen atoms as well as two oxygen atoms. The oxygen atoms are very strong oxidizing agents therefore in order to break this substrate down it must undergo oxidation. This can be done
In this experiment, four elimination reactions were compared and contrasted under acidic (H2SO4) and basic (KOC(CO3)3) conditions. The acid-catalyzed dehydration was done on 2-butanol and 1-butanol; a 2ᵒ and 1ᵒ alcohol, respectively. The base-induced dehydrobromination was performed on 2-bromobutane and 1-bromobutane; isomeric halides. The stereochemistry and regiochemistry of the four reactions were analyzed by gas chromatography (GC) to determine product distribution (assuming that the amount of each product in the gas mixture is proportional to the area under its complementary GC peak. The three butene products have been verified that they elute in the following order: 1-butene, trans-2-butene, and cis-2-butene.
The Effect of Temperature of Hydrochloric Acid on the Rate of Reaction Between Hydrochloric Acid and Magnesium
The Effect of Concentration of Hydrochloric Acid on the Rate of Reaction with Magnesium Aim: To investigate the effect of concentration of hydrochloric acid on the rate of reaction with magnesium Prediction: As the concentration of the hydrochloric acid increases, so will the rate of reaction Hypothesis: In a reaction, particles of two different reactants react together to form a product. The reaction only takes place on account of two things, if the particles collide, and if the collision has enough 'activation energy'. The two reactant particles, in this case magnesium particles and hydrochloric acid particles, must collide with each other on the correct 'collision course'. If this does not occur then no chemical reaction will take place. The reaction must also have enough energy, this can be affected by temperature, the more heat the particles have the faster they move and so the more energy therefore more chance of successful collisions.
U.S. Chemical Safety and Hazard Investigation Board. (March 20, 2007). Final Investigation Report. Retrieved July 26, 2010, from U.S. Chemical and Safety Board: http://www.csb.gov/assets/document/CSBFinalReportBP.pdf
Missouri Department Of Health And Senior Services Section For Environmental Public Health. 2014. Swimming Pool and Spa Water Chemistry. [e-book] Missouri: nitt.edu. p. 14, 15. Available through: nitt.edu http://www.nitt.edu/home/students/facilitiesnservices/sportscenter/swimmingpool/Swim-pool-chemistry.pdf [Accessed: 30 Mar 2014].
Investigating the Effects of Temperature on the Rate of Reaction between Magnesium and Hydrochloric Acid
Plontke, R. (2003, March 13). Chemnitz UT. TU Chemnitz: - Technische Universität Chemnitz. Retrieved April 1, 2014, from http://www.tu-chemnitz.de/en/