DOCSLIB.ORG

Energetic Materials

Total Page：16

File Type：pdf, Size：1020Kb

Download full-text PDF Read full-text
Energetic Materials DISSERTATION ZUR ERLANGUNG DES DOKTORGRADES DER FAKULTÄT FÜR CHEMIE UND PHARMAZIE DER LUDWIG-MAXIMILIANS-UNIVERSITÄT MÜNCHEN Synthesis, Characterization, Scale-up and Investigation of Structure-property Relationships of High Energy Density Materials Dominik Ernst Dosch aus Wertheim, Deutschland 2021 Erklärung: Diese Dissertation wurde im Sinne von § 7 der Promotionsordnung vom 28. November 2011 von Herrn Professor Dr. Thomas M. Klapötke betreut. Eidesstattliche Versicherung: Diese Dissertation wurde eigenständig und ohne unerlaubte Hilfe erarbeitet. München, den 23 März 2021 __________________ Dominik Dosch Dissertation eingereicht am: 24. März 2021 1. Gutachter: Prof. Dr. Thomas M. Klapötke 2. Gutachter: Prof. Dr. Konstantin Karaghiosoff Mündliche Prüfung am: 29.04.2021 Danksagung An erster Stelle gilt mein Dank meinem Doktorvater Prof. Dr. Thomas M. Klapötke für die freundliche Aufnahme in seinen Arbeitskreis und die interessante Themenstellung für meine Promotion. Außerdem möchte ich mich für die stetige finanzielle und fachliche Unterstützung meiner persönlichen Forschungsvorhaben sowie für seine Begeisterung für die Erforschung hochenergetischer Materialien bei ihm bedanken und nicht zuletzt für das Vertrauen, welches er beim EURENCO Projekt in mich und meine Fähigkeiten als Chemiker gesetzt hat. Herrn Prof. Dr. Konstantin Karaghiosoff danke ich nicht nur für die freundliche Übernahme des Zweitgutachtens dieser Dissertation, sondern auch für seinen unermüdlichen Einsatz für das IT-Team und das X-Ray Team. Seine Anmerkungen und Korrekturen zu diversen Publikationen waren für mich von unschätzbarem Wert und durch seine freundliche und offene Art konnte er mich auch in schwierigen Phasen immer motivieren. Dafür möchte ich dir meinen Dank aussprechen Conny! Ich hoffe, dass das IT Team auch bei künftigen Raubzügen zum LRZ weiterhin fette Beute macht. Der Prüfungskommission, bestehend aus Prof. Dr. T. M. Klapötke, Prof. Dr. K. Karaghiosoff, Prof. Dr. H. C. Böttcher, Prof. Dr. A. Kornath, Prof. Dr. I. Ivanović- Burmazović und Prof. Dr. O. Trapp danke ich für Ihre Zeit und die Bereitschaft zur Bildung der selbigen. Herrn Dr. Burkhard Krumm danke ich für die gute Betreuung beim EURENCO Projekt, für interessante Anregungen und Diskussionen auch fernab der Chemie, sowie für die Aufnahme zahlreicher NMR Spektren. Bei Herrn Dr. Jörg Stierstorfer möchte ich mich vor allem dafür bedanken, dass er mich bei verschiedenen Projekten sowohl fachlich als auch persönlich herausfordern konnte und mir auf diese Weise eine große Hilfe in meiner Entwicklung als Wissenschaftler war. Durch seine unnachahmliche Art, ist er ein elementarer Bestandteil dieses Arbeitskreises und durch niemanden zu ersetzen. Frau Irene Scheckenbach danke ich für Ihr herausragendes organisatorisches Talent und Ihre Unterstützung bei sämtlichen bürokratischen Angelegenheiten. Eine gute Seele wie Sie im Arbeitskreis zu haben ist Gold wert und ich hoffe für meine Nachfolger, dass sie dieser Funktion noch lange nachgehen kann. Allen während meiner Promotionsdauer anwesenden Kollegen im Arbeitskreis danke ich für die stets sehr gute und freundschaftliche Arbeitsatmosphäre. In möchte mich bei Herrn Dr. Marco Reichel für die gute Zusammenarbeit bei diversen Projekten und Publikationen bedanken. Allen Mitstreitern aus Labor D.3.103 gilt mein besonderer Dank, namentlich Stefan Huber, Alicia Dufter-Münster, Christin Kirst, Alexander Schweiger, Jonathan Tietze und Dr. Sarah Linert. Wir hatten eine großartige Zeit im Labor und ich hoffe, dass euch die Marschmusikmontage, die Cantina-Band, Sputnik Booster, das Bananaphone und der YEE-Dino in Zukunft fehlen werden. I Bei meinen Mentoren aus den beiden Abschlussarbeiten und meinen F-Praktika möchte ich mich ebenfalls bedanken, namentlich bei Dr. Tomasz Witkowski, Dr. Johann Glück, Dr. Johannes Broichhagen, Dr. Oliver Pham-Schönwetter und Dr. Arno Hahma. Ihr alle habt auf eure individuelle Art und Weise einen Beitrag dazu geleistet meine präparativen und fachlichen Fähigkeiten auszubauen und zu verfeinern – Dafür ein herzliches Dankeschön! Mein weiterer Dank gilt meinem F-Praktikanten Daniel Bauer sowie meiner Bachelorandin Veronika Fuchs. Durch ihre präparativen Tätigkeiten und die Mitarbeit konnten beide in erheblichem Maße zu meiner letzten Publikation für diese kumulative Dissertation beitragen. Beide werden ihren Weg in der Wissenschaft erfolgreich gehen und ich schätze sie als ausgezeichnete Chemiker & Kollegen. Bei meinen besten Freunden Max Born, Sebastian Birkholz, Johannes Guilleaume, Christoph Dengel, Thomas Metz, Tobias Fäth und Jörn Dietze möchte ich mich ebenso für Ihre Unterstützung bedanken. Ein Mensch ist nur dann wirklich reich gesegnet, wenn er Freunde wie euch hat, die ihm stets zur Seite stehen, in guten wie in schlechten Tagen! Nicht zuletzt gilt mein Dank meiner Familie, im Besonderen meinen Eltern Ernst und Gisela, sowie meinen Geschwistern Isabell und Christopher. Durch euren unermüdlichen Glauben daran, dass ich alles schaffen kann was ich mir vornehme und durch euren Einsatz für meinen persönlichen Bildungsweg bin ich euch für immer zum Dank verpflichtet. Nicht zu vergessen sind meine Großeltern Irmgard und Bruno, meine Tante Helga, mein Patenonkel Edgar meine „Kosengine“ Alice und die übrigen Ludwigshäfner. Ihr alle seid mir ein einzigartiger Rückhalt im Leben und habt mich von Kindesbeinen an mit allen euch zur Verfügung stehenden Mitteln gefördert und entwickelt. Ohne euren jeweiligen Einfluss, wäre ich heute nicht der Mensch der ich bin und dafür möchte ich mich bei euch allen bedanken, denn ohne euren individuellen Anteil wäre diese Arbeit nicht möglich gewesen. II Table of Contents 1 Introduction ........................................................................................................ - 1 - 1.1 Energetic Materials ........................................................................................... - 1 - 1.1.1 Classification of high energy density materials (HEDMs) ................... - 1 - 1.1.2 Thermostable secondary explosives & booster explosives ................. - 3 - 1.1.3 High energy density oxidizers (HEDOs) for propellants ...................... - 5 - 1.2 Hirshfeld Surface Analysis ................................................................................ - 7 - 1.2.1 Hirshfeld Surface Analysis (HSA) – A short Introduction .................... - 7 - 1.2.2 Safety assessment of energetic materials via HSA ............................ - 9 - 1.3 Motivation and Objectives ............................................................................... - 10 - 1.4 References ..................................................................................................... - 11 - 2 Summary and Conclusion .............................................................................. - 14 - 2.1 An Optimized & Scaled-Up Synthetic Procedure for Trinitroethyl Formate TNEF .............................................................................................................. - 14 - 2.2 Scalability of a Time- and Cost-Effective Procedure for the Synthesis of Picryl Bromide................................................................................................. - 14 - 2.3 Correlation between Structure and Energetic Properties of Three Nitroaromatic Compounds: Bis(2,4-dinitrophenyl) Ether, Bis(2,4,6- trinitrophenyl) Ether, and Bis(2,4,6-trinitrophenyl) Thioether .......................... - 15 - 2.4 Investigation of Structure-Property Relationships of Three Nitroaromatic Compounds: 1-Fluoro-2,4,6-trinitrobenzene, 2,4,6-Trinitrophenyl methanesulfonate, and 2,4,6-Trinitrobenzaldehyde. ....................................... - 16 - 2.5 A Study of 3,5-Dinitro-1-(2,4,6-trinitrophenyl)-1H-pyrazol-4-amine (PicADNP) as a New High Energy Density Booster Explosive ....................... - 17 - 3 An Optimized & Scaled-Up Synthetic Procedure for Trinitroethyl Formate TNEF ................................................................................................................. - 18 - 3.1 Abstract .......................................................................................................... - 18 - 3.2 Introduction ..................................................................................................... - 18 - 3.3 Experimental Section ...................................................................................... - 19 - 3.4 Results and Discussion .................................................................................. - 21 - 3.4.1 Synthesis .......................................................................................... - 21 - 3.4.2 Spectroscopic Characterization and Elemental Analysis .................. - 21 - 3.4.3 Sensitivity Assessment ..................................................................... - 22 - 3.4.4 Thermal Analysis .............................................................................. - 22 - 3.4.5 Storage and Short Term Stability Test .............................................. - 23 - 3.5 Conclusion ...................................................................................................... - 23 - III 3.6 Acknowledgements......................................................................................... - 23 - 3.7 References ..................................................................................................... - 24 - 3.8 Supporting Information ................................................................................... - 25 - 4 Scalability of a Time-
Load more

Recommended publications
  • PHD-12-MCATEER (2).Pdf
    CRANFIELD UNIVERSITY Daniel McAteer The Development of Novel, Low Sensitivity, Gas-generating Formulations for Hotwire Ignited Devices Department of Engineering and Applied Science PhD Academic Year: 2012 - 2013 Supervisors: Professor J Akhavan & Dr A Contini April 2013 CRANFIELD UNIVERSITY DEAS PhD Academic Year 2012 - 2013 Daniel McAteer The Development of Novel, Low Sensitivity, Gas-generating Formulations for Hotwire Ignited Devices Supervisors: Professor J Akhavan & Dr A Contini April 2013 © Cranfield University 2013. All rights reserved. No part of this publication may be reproduced without the written permission of the copyright owner. Abstract A novel, low sensitivity, gas-generating composition was developed to replace an existing primary explosive, potassium picrate, for use in a generic squib device. The novel composition was based on energetic materials researched from the open literature. The chosen materials were synthesised or purchased and combined in order to produce formulations which would reproducibly ignite when contacted with a hotwire. The formulations were assessed for their chemical compatibility and homogeneity by small-scale hazard testing, differential scanning calorimetry (DSC) and nuclear magnetic resonance (NMR) spectroscopy. The compositions were test fired within squibs coupled to a pressure bomb and the pressure generation and rise time was measured using a piezoelectric gauge. Keywords: Squib, Bridgewire, Electroexplosive Device, Igniter i Acknowledgements I was able to pursue this PhD thanks to the support and encouragement provided by my parents, without them I would not have made it this far. A courtesy note is included for my brother and sisters who, although thoroughly uninterested in my research, were present throughout my studies and offered support of a sort.
    [Show full text]
  • System Documentation
    TOXICS RELEASE INVENTORY DATA DELIVERY SYSTEM TRI-DDS 2001 System Documentation Prepared for: DoD EPCRA TRI Working Group Prepared by: URS Corporation 1093 Commerce Park Drive, Suite 100 Oak Ridge, Tennessee 37830 Doc #F9906181.MW97 April 2002 Please Note: The following distribution restriction applies only to the TRI-DDS Software. It does not apply to this document. Distribution authorized to the Department of Defense and U.S. DoD contractors only to protect technical or operational data or information from automatic dissemination under the International Exchange Program or by other means (effective 7 February 2002). Other requests shall be referred to the Deputy Undersecretary of Defense, Installation and Environment [DUSD(I&E)]. WARNING - This document contains technical data whose export is restricted by the Arms Export Control Act (Title 22, U.S.C., Sec 2751, et seq.) or the Export Administration Act of 1979, as amended, Title 50, U.S.C., App. 2401 et seq. Violations of these export laws are subject to severe criminal penalties. Disseminate in accordance with provisions of DoD Directive 5230.25. Destroy by any method that will prevent disclosure of contents or reconstruction of the document. Table of Contents List of Tables.........................................................................................................................v Chapter 1 OVERVIEW ...........................................................................................................................1-1 1.1 Background ......................................................................................................................1-3
    [Show full text]
  • WO 201 1/056841 Al
    (12) INTERNATIONAL APPLICATION PUBLISHED UNDER THE PATENT COOPERATION TREATY (PCT) (19) World Intellectual Property Organization International Bureau (10) International Publication Number ι (43) International Publication Date ¾ ί t 12 May 2011 (12.05.2011) WO 201 1/056841 Al (51) International Patent Classification: (81) Designated States (unless otherwise indicated, for every C07C 213/02 (2006.01) C07D 271/12 (2006.01) kind of national protection available): AE, AG, AL, AM, AO, AT, AU, AZ, BA, BB, BG, BH, BR, BW, BY, BZ, (21) International Application Number: CA, CH, CL, CN, CO, CR, CU, CZ, DE, DK, DM, DO, PCT/US2010/055248 DZ, EC, EE, EG, ES, FI, GB, GD, GE, GH, GM, GT, (22) International Filing Date: HN, HR, HU, ID, IL, IN, IS, JP, KE, KG, KM, KN, KP, 3 November 2010 (03.1 1.2010) KR, KZ, LA, LC, LK, LR, LS, LT, LU, LY, MA, MD, ME, MG, MK, MN, MW, MX, MY, MZ, NA, NG, NI, (25) Filing Language: English NO, NZ, OM, PE, PG, PH, PL, PT, RO, RS, RU, SC, SD, (26) Publication Language: English SE, SG, SK, SL, SM, ST, SV, SY, TH, TJ, TM, TN, TR, TT, TZ, UA, UG, US, UZ, VC, VN, ZA, ZM, ZW. (30) Priority Data: 61/257,721 3 November 2009 (03.1 1.2009) U S (84) Designated States (unless otherwise indicated, for every kind of regional protection available): ARIPO (BW, GH, (71) Applicant (for all designated States except US): PACIF¬ GM, KE, LR, LS, MW, MZ, NA, SD, SL, SZ, TZ, UG, IC SCIENTIFIC ENERGETIC MATERIALS COM¬ ZM, ZW), Eurasian (AM, AZ, BY, KG, KZ, MD, RU, TJ, PANY [US/US]; 7073 W .
    [Show full text]
  • Making Plastic Explosives from Bleach by the Jolly Roger Potassium
    Making Plastic Explosives from Bleach by The Jolly Roger Potassium chlorate is an extremely volatile explosive compound, and has been used in the past as the main explosive filler in grenades, land mines, and mortar rounds by such countries as France and Germany. Common household bleach contains a small amount of potassium chlorate, which can be extracted by the procedure that follows. First off, you must obtain: 1.A heat source (hot plate, stove, etc.) 2.A hydrometer, or battery hydrometer 3.A large Pyrex, or enameled steel container (to weigh chemicals) 4.Potassium chloride(sold as a salt substitute at health and nutrition stores) Take one gallon of bleach, place it in the container, and begin heating it. While this solution heats, weigh out 63 grams of potassium chloride and add this to the bleach being heated. Constantly check the solution being heated with the hydrometer, and boil until you get a reading of 1.3. If using a battery hydrometer, boil until you read a FULL charge. Take the solution and allow it to cool in a refrigerator until it is between room temperature and 0øC. Filter out the crystals that have formed and save them. Boil this solution again and cool as before. Filter and save the crystals. Take the crystals that have been saved, and mix them with distilled water in the following proportions: 56 grams per 100 milliliters distilled water. Heat this solution until it boils and allow to cool. Filter the solution and save the crystals that form upon cooling. This process of purification is called "fractional crystallization".
    [Show full text]
  • Ammunition) to Manual Small Arms 2.1
    Chapter 2 THEORETICAL AND LEGAL SUPPORT OF CRIMINALISTIC RESEARCH OF CARTRIDGES (AMMUNITION) TO MANUAL SMALL ARMS 2.1. Cartridges (ammunition) as objects criminalistic research (concept, essence, classification) Currently, one of the unresolved problems of assessing the conclu- sion of forensic ballistic examination is the use in its content of terms and their definitions that do not meet modern scientific ideas about the objects under study. This applies to both legislative acts and normative legal acts regulating the conduct of relevant examinations, in particular the study of cartridges (ammunition) used for shooting from small arms, traces of their use. However, the accuracy and unambiguity of terminol- ogy used in forensic ballistic examination of cartridges (ammunition) are important to ensure its uniform understanding and use in both foren- sic and law enforcement activities. It is no coincidence that the literature emphasizes that one of the main elements of the concept of the General theory of forensic examina- tion is the doctrine of the means and forms of communicative activity in the production of forensic examinations; the Central part of this element is the language of the expert, the system of expert concepts and terms designating them. The development and improvement of the General theory of forensic examination largely depend on the development and improvement of its conceptual apparatus, in-depth disclosure of the es- sence of objects, phenomena reflected in each concept [3, p. 103]. R. S. Belkin notes that the introduction of new terms and their definitions into forensic examination as a specific sphere of scientific knowledge is carried out by expanding the existing basis of theoretical provisions and empirical data [36, p.
    [Show full text]
  • FSTC 381-5042, Handbook of Foreign Explosives
    U. S. ARMY MATERIEL COMMAND FSIC 381-5042 HANDBOOK OF FOREIGN EXPLOSIVES U.S. Army Foreign Science and Technology Center Munitions Building, Washington, D.C. 20315 FSTC 381-5CA-2 is published for the information and guidance of all concerned. Comments, and requests for additional copies, should he sent to the Commanding Officer, at the above address. A Category I Intelligence Document. This document was compiled and pro­ ducted by the U.S. Army Foreign Science and Technology Center and is intended for rise within the U.S. Army Materiel Command. This document has not been approved by the Office of the Assistant Chief of Staff for Intelligence and therefore does not necessarily represent agreed Depart­ ment of the Army intelligence. DESCRIPTORS Explosives: manufacturing, testing, use, characteristics, loading, com­ parison, strength power, brisance, composition; pyrotechnics; bursting charge; propelling charge; high-explosive ammunition. Project Eld 596 FSTC 381-5042 HANDBOOK OF FOREIGN EXPLOSIVES October 1965 (Based on information available as of June 1964) Prepared by Picatinny Arsenal Dover, New Jersey 07801 for ' U.S. Army Foreign Science and Technology Center Munitions Building Washington, D. C . 20315 ABSTRACT (u) This Handbook of Foreign Explosives contains technical information and reference data on the chemical and physical character­ istics, known variations in nomenclature, and the application of explosive compounds to the various types of ammunition in use by selected countries. TABLE OF CONTENTS Dago Section I. INTRODUCTION ' Purpose _ ^ Scope ' ^ Summary • g Section II. GENERAL INDEX y Section III. COUNTRY INDEX . Belgium France • P q -^ Germany 2U3 Italy 3-17 Japan 360 Soviet Union 388 Spain 429 Sweden .
    [Show full text]
  • Chemical Weapons Convention, the United States May Require Special Declarations Related to Chemical Shipments Under Either the ITAR Or the EAR
    Appendix 1 Unit Table A.1. Conversion Factors Overview The International System of Units (SI) is a modernized version of the metric system established by international agreement. The metric system of measurement was developed during the French Revolution and was first promoted in the U.S. by Thomas Jefferson. Its use was legalized in the U.S. in 1866. In 1902, proposed congressional legislation requiring the U.S. Government to use the metric system exclusively was defeated by a single vote. SI provides a logical and interconnected framework for all measurements in science, industry, and commerce. The metric system is much simpler to use than the existing English system since all its units of measurement are divisible by 10. Conversion Factors The following list provides the conversion relationship between U.S. customary units and SI (International System) units. The proper conversion procedure is to multiply the specified value on the left (primarily U.S. customary values) by the conversion factor exactly as given below and then round to the appropriate number of significant digits desired. For example, to convert 11.4 ft to m: 11.4 Â 0.3048 = 3.47472, which rounds to 3.47 m. Do not round either value before performing the multiplication, as accuracy would be reduced. A complete guide to the SI system and its use can be found in ASTM E 380, Metric Practice. Select this link for an explanation of WSDOT's foot to meter conversion method (http://www.wsdot.wa.gov/Reference/metrics/foottometer.htm). Note that Convert.exe (http://www.wsdot.wa.gov/NR/rdonlyres/4A1238B7- 69FC-434E-8BF0-317AA149F5C0/0/convert.exe) uses the 1959 conversion fac- tors for distance (http://www.wsdot.wa.gov/Reference/metrics/foottometer.htm) i.e.
    [Show full text]
  • United States Patent (19) (11 3,712,223 Degn (45) Jan
    United States Patent (19) (11 3,712,223 Degn (45) Jan. 23, 1973 (54) PYROTECHNIC, WHISTLE, AND 3,093,523 6, 1963 Besser ................................ 49/99 X METHOD OF MAKENG 3,103,458 9, 1963 Besser et al.... ... 149/99 X (76 Inventor: Ralph G. Degn, 214 A Universitya 3,309.2503,228,815 3/1967l/1966 FaltermanHenry et al.......... et al... ... 149799 49.42 X Village, Salt Lake City, Utah 84108 3,396,060 8/1968 Piccone.................................. 149 fa2 22 Filed: Oct. 7, 1970 Primary Examiner-Stephen J. Lechert, Jr. (21) Appl. No.: 78,921 Attorney-H. Ross Workman 52 U.S. C. ........................ 102/31, 149/38, 149/39, 57) ABSTRACT 149/40, 149/41, 149142, 149/43, 14.9144 A pyrotechnic whistle and method of producing same (51 int. C. ............................................... CO6d 1100 which prevents a minimum danger of explosion 58 Field of Search ...... 102/3 l; 149/42, 44, 114, 85, formed of a tubular reaction chamber and a 149/38, 39, 40, 41, 43 pyrochemical mixture formed by mixing together a salt of salicylic acid and an oxidizing agent. Finely di 56 References Cited vided titanium is added to the pyrochemical mixture UNITED STATES PATENTS or to other pyrochemical mixtures formed of aromatic acids and oxidizing agents to provide a trail of glitter 3,033,715 5, 1962 Preckel............................... 149/99 X when the pyrochemical mixture reacts. 3,033,718 5f 1962 Preckel... ... 149/99 X 3,088,858 5/963 Camp................................. 149/99 X 10 Claims, No Drawings 3,712,223 1. 2 PYROTECHNEC, WHISTLE, AND METHOD OF very expensive.
    [Show full text]
  • Rules and Regulations Governing Schools in the State of Colorado
    COLORADO DEPARTMENT OF PUBLIC HEALTH AND ENVIRONMENT Division of Environmental Health and Sustainability 6 CCR 1010-6 RULES AND REGULATIONS GOVERNING SCHOOLS IN THE STATE OF COLORADO TABLE OF CONTENTS 6.1 Authority .......................................................................................................................................... 2 6.2 Scope and Purpose........................................................................................................................... 2 6.3 Applicability ..................................................................................................................................... 2 6.4 Definitions ........................................................................................................................................ 3 6.5 Incorporation by Reference ............................................................................................................. 7 6.6 Compliance Procedures ................................................................................................................... 7 6.6.1 Inspections ............................................................................................................................. 7 6.6.2 Self-Certification..................................................................................................................... 8 6.6.3 Compliance Assurance ........................................................................................................... 9 6.6.4 Variance Procedures ...........................................................................................................
    [Show full text]
  • (12) United States Patent (10) Patent No.: US 8.404,897 B2 Fronabarger Et Al
    USOO8404897B2 (12) United States Patent (10) Patent No.: US 8.404,897 B2 Fronabarger et al. (45) Date of Patent: Mar. 26, 2013 (54) FACILE SYNTHESIS OF 3-AMINOPICRIC OTHER PUBLICATIONS ACD International Preliminary Report on Patentability dated May 18, (75) Inventors: John W. Fronabarger, Sun Lakes, AZ R A. NS E. NWAA.R 2011 SS Michael D. Williams,O O Gilbert, AZ in relatedOla Application SeaC eportNo. PCT/US2010/055248, an ritten Upinion pp.e 1-3.e. (US) Borsche and Feske, “Uber den wechselseitigen Austausch von (73) Assignee: Pacific Scientific Energetic Materials Licensitytisch gebund Hvolroxvil oxy und Halalogen , ChemischeSe Company, Chandler, AZ (US) Katritzky. et al., “Direct Amination of Nitrogenzenes by Vicarious Nucleophilic Substitution.” Journal of Organic Chemistry, (*) Notice: Subject to any disclaimer, the term of this 51(25):5039-5040 (1986). patent is extended or adjusted under 35 Makosza, et al., “Vicarious Nucleophilic Substitution of Hydrogen.” U.S.C. 154(b) by 110 days. Acc. Chem. Res., 20:282-289 (1987). Mitchell, et al., A Versatile Synthesis of 1,3,5-Triamino-2,4,6- (21) Appl. No.: 12/939,012 Trinitrobenzene (TATB), 37" International Institute of Chemical Technology (ICT) Conference, Karlsruhe, Germany (2006). (22) Filed: Nov. 3, 2010 Pagoria, et al., “1,1,1-Trimethylhydrazinium Iodide: A Novel, Highly Reactive Reagent for Aromatic Amination via Vicarious (65) Prior Publication Data Nucleophilic Substitution of Hydrogen.” J. Org. Chem... 61 :2934 US 2011 FO1058OO A1 Mayay 5,, 2011 2935 (1996). * cited by examiner Related U.S. Application Data (60) final application No. 61/257,721, filed on Nov.
    [Show full text]
  • 3. Making Plastic Explosives from Bleach by the Jolly Roger
    3. Making Plastic Explosives from Bleach by The Jolly Roger Potassium chlorate is an extremely volatile explosive compound, and has been use d in the past as the main explosive filler in grenades, land mines, and mortar rounds by such countries as France and Germany. Common househo ld bleach contains a small amount of potassium chlorate, which can be extracted by the procedure that follows. First off, you must obtain: 1.A heat source (hot plate, stove, etc.) 2.A hydrometer, or battery hydrometer 3.A large Pyrex, or enameled steel container (to weigh chemicals) 4.Potassium chloride(sold as a salt substitute at health and nutrition stores) Take one gallon of bleach, place it in the container, and begin heating it. Whil e this solution heats, weigh out 63 grams of potassium chloride and add this to the bleach being heated. Constantly check the solution being heated with the hydrometer, and boil until you get a reading of 1.3. If using a battery hydrometer, boil until you read a FULL charge. Take the solution and allow it to cool in a refrigerator until it is between roo m temperature and 0øC. Filter out the crystals that have formed and save them. Boil this solution again and cool as before. Filter and save the crys tals. Take the crystals that have been saved, and mix them with distilled water in the following proportions: 56 grams per 100 milliliters distilled water. Heat this solution until it boils and allow to cool. Filter the solution and save the crystals that form upon cooling.
    [Show full text]
  • Determination of Surfactants from Foam-Formed Products
    Determination of surfactants from foam-formed products Master’s Thesis University of Jyväskylä Department of Chemistry 15.10.2018 Janika Viitala i ABSTRACT In this Master’s thesis, determination of surfactant residues from solid foam-formed samples was studied. The residues of an anionic surfactant, sodium dodecyl sulphate (SDS), and a non- ionic surfactant Tween 20 (polyoxyethylenesorbitan monolaurate), were determined from foam-formed hand sheets. The measured surfactant residues were compared with the theoretical values calculated from the water content of the sample before drying phase and the surfactant dosage. In addition to analysis of surfactant residues, determination of 4- dodecylbenzenesulphonic acid (4-DBSA, anionic surfactant) in water solution by UV spectrophotometry was studied. The literature part considers the chemistry of surfactants and introduces the relatively new concept of papermaking, foam forming. The main focus in the literature part is in the analysis methods of surfactants. Sample pre-treatment methods and the use of spectrophotometry, chromatography and atomic spectroscopy in the determination of surfactants are discussed. In addition, the chemical legislation, toxicological concerns of surfactants and the regulations concerning paper and board in food contact materials are discussed. To determine surfactant residues, two different determination methods were used for both surfactants. SDS residues were determined by spectrophotometry and by inductively coupled plasma optical emission spectrometry (ICP-OES). Tween 20 residues were determined by spectrophotometry and by high-performance liquid chromatography equipped with a diode array detector (HPLC-DAD). Ultrasound-assisted nitric acid digestion was used as a sample preparation method for the ICP-OES analysis. Before the chromatographic determination, Tween 20 was extracted from the sample by methanol in Soxhlet extraction.
    [Show full text]