Federal Register/Vol. 67, No. 229/Wednesday, November 27
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Optimization of Ammonium Sulfamate Nitration for the Preparation of Ammonium Dinitramide
Optimization of Ammonium Sulfamate Nitration for the Preparation... 83 Central European Journal of Energetic Materials, 2014, 11(1), 83-97 ISSN 1733-7178 Optimization of Ammonium Sulfamate Nitration for the Preparation of Ammonium Dinitramide Alok Kumar MANDAL*1, Ganesh Murlidhar KUNJIR1, Jaivindra SINGH1, Sushma S. ADHAV1, Sunil Kumar SINGH1, Raj Kishore PANDEY1, Bikash BHATTACHARYA1, Mannepalli LAKSHMI KANTAM2 and Karasala Vijaya KUMAR2 1High Energy Materials Research Laboratory, Chemical Engineering and Pilot Plant Division, Sutarwadi, Pune-411021, India 2Indian Institute of Chemical Technology, Hyderabad-500 007, India *E-mail: [email protected] Abstract: The reaction kinetics for the preparation of ammonium dinitramide (ADN) is described. ADN is the ammonium salt of the dinitramide anion, and belongs to the group of inorganic oxidizers, mainly useful for energetic rocket propellant formulations, particularly for underwater applications. It is also a potential candidate to replace ammonium perchlorate (AP), in order to develop chlorine-free, green propellants. At HEMRL, ADN is prepared by the nitration of ammonium sulfamate (AS) using mixed acid, followed by hydrolysis, neutralization with ammonia (g) and rectification using solvent. The nitration of ammonium sulfamate (AS) is carried out at a subzero temperature of -40 ±1 °C. The yield of ADN is reliant on the formation of dinitramidic acid, an intermediate product formed during the hydrolysis step, and its stability is predominantly dependent upon the level of acidity and temperature of the reaction medium. Prior to these kinetics studies, process optimization of the nitration of ammonium sulfamate (AS) was performed and gave the final mole ratio of AS:HNO3:H2SO4. Since the nitration of AS is sensitive to temperature, the rate of reaction was studied at fixed temperatures with variation of time, keeping all of the other parameters, such as vessel volume, agitator speed, feed rate etc., constant. -
Stabilization of the New Oxidizer Ammonium Dinitramide (ADN) in Solid Phase
NATO UNCLASSIFIED Stabilization of the New Oxidizer Ammonium Dinitramide (ADN) in Solid Phase Dr. Manfred Bohn Fraunhofer-Institut für Chemische Technologie (ICT) Postfach 1240 D-76318 Pfinztal-Berghausen GERMANY e-mail: [email protected] ABSTRACT Ammonium dinitramide (ADN) is one of the substances, which are seen to be able to replace ammonium perchlorate (AP) as oxidizer in rocket propellants. Some of the performance data in comparison to AP substantiate this suggestion (values for AP in brackets). It has a good oxygen balance of +25.8% (+34%), a more positive enthalpy of formation, -1208 J/g (-2518 J/g) and a higher heat of explosion as AP, 3337 J/g (1972 J/g). An additional advantage is that the reaction products of ADN are free of signature. One drawback of ADN clearly is the much lower thermal stability than that of AP, together with the relatively low melting point between 92 and 94°C. But the lower stability must not exclude its application in some types of rocket systems. The intrinsic stability of ADN is not much lower than that of unstabilized nitrocellulose. If it would be possible to find stabilizers, ADN can be considered as a substitute candidate for AP. An extensive investigation was made with eight substances to find out their stabilization effect on ADN. The ADN samples were mixed intensively with an amount of 2 mol-% each of these chemicals. The experimental methods used to determine the stabilization effect have been mass loss as function of time and temperature, 65°C, 70°C, 75°C, 80°C, and adiabatic self heating. -
A Guide to Export Controls
Foreign Affairs, Trade and Affaires étrangères, Commerce et Development Canada Développment Canada A Guide To CANADA’S EXPORT CONTROLS December 2012 Introduction The issuance of export permits is administered by the Export Controls Division (TIE) of Foreign Affairs, Trade and Development Canada (DFATD). TIE provides assistance to exporters in determining if export permits are required. It also publishes brochures and Notices to Exporters that are freely available on request and on our website www.exportcontrols.gc.ca. How to contact us: Export Controls Division (TIE) Foreign Affairs, Trade and Development Canada 111 Sussex Drive Ottawa, Ontario K1A 0G2 Telephone: (613) 996-2387 Facsimile: (613) 996-9933 Email: [email protected] For information on how to apply for an export permit and additional information on export controls please refer to our website. To enquire on the status of an export permit application: Recognized EXCOL users can check the status of an export permit application on-line. Non-recognized users can call (613) 996-2387 or email [email protected] and quote your export permit application identification (ref ID) number. Export Controls Division website: www.exportcontrols.gc.ca This Guide, at time of publication, encompasses the list of items enumerated on the Export Control List (ECL) that are controlled for export in accordance with Canadian foreign policy, including Canada’s participation in multilateral export control regimes and bilateral agreements. Unless otherwise specified, the export controls contained in this Guide apply to all destinations except the United States. Canada’s Export Control List can be found at the Department of Justice website at http://canada.justice.gc.ca/. -
Aldrich Vapor
Aldrich Vapor Library Listing – 6,611 spectra This library is an ideal tool for investigator using FT-IR to analyze gas phase materials. It contains gas phase spectra collected by Aldrich using a GC-IR interface to ensure chromatographically pure samples. The Aldrich FT-IR Vapor Phase Library contains 6,611 gas phase FT-IR spectra collected by Aldrich Chemical Company using a GC interface. The library includes compound name, molecular formula, CAS (Chemical Abstract Service) registry number, Aldrich catalog number, and page number in the Aldrich Library of FT-IR Spectra, Edition 1, Volume 3, Vapor-Phase. Aldrich Vapor Index Compound Name Index Compound Name 6417 ((1- 3495 (1,2-Dibromoethyl)benzene; Styrene Ethoxycyclopropyl)oxy)trimethylsilane dibromide 2081 (+)-3-(Heptafluorobutyryl)camphor 3494 (1-Bromoethyl)benzene; 1-Phenylethyl 2080 (+)-3-(Trifluoroacetyl)camphor bromide 262 (+)-Camphene; 2,2-Dimethyl-3- 6410 (1-Hydroxyallyl)trimethylsilane methylenebicyclo[2.2.1]heptane 6605 (1-Methyl-2,4-cyclopentadien-1- 2828 (+)-Diisopropyl L-tartrate yl)manganese tricarbonyl 947 (+)-Isomenthol; [1S-(1a,2b,5b)]-2- 6250 (1-Propynyl)benzene; 1-Phenylpropyne Isopropyl-5-methylcyclohexano 2079 (1R)-(+)-3-Bromocamphor, endo- 1230 (+)-Limonene oxide, cis + trans; (+)-1,2- 2077 (1R)-(+)-Camphor; (1R)-(+)-1,7,7- Epoxy-4-isopropenyl-1- Trimethylbicyclo[2.2.1]heptan- 317 (+)-Longifolene; (1S)-8-Methylene- 976 (1R)-(+)-Fenchyl alcohol, endo- 3,3,7-trimethyltricyclo[5.4.0 2074 (1R)-(+)-Nopinone; (1R)-(+)-6,6- 949 (+)-Menthol; [1S-(1a,2b,5a)]-(+)-2- Dimethylbicyclo[3.1.1]heptan-2- -
Aldrich Raman
Aldrich Raman Library Listing – 14,033 spectra This library represents the most comprehensive collection of FT-Raman spectral references available. It contains many common chemicals found in the Aldrich Handbook of Fine Chemicals. To create the Aldrich Raman Condensed Phase Library, 14,033 compounds found in the Aldrich Collection of FT-IR Spectra Edition II Library were excited with an Nd:YVO4 laser (1064 nm) using laser powers between 400 - 600 mW, measured at the sample. A Thermo FT-Raman spectrometer (with a Ge detector) was used to collect the Raman spectra. The spectra were saved in Raman Shift format. Aldrich Raman Index Compound Name Index Compound Name 4803 ((1R)-(ENDO,ANTI))-(+)-3- 4246 (+)-3-ISOPROPYL-7A- BROMOCAMPHOR-8- SULFONIC METHYLTETRAHYDRO- ACID, AMMONIUM SALT PYRROLO(2,1-B)OXAZOL-5(6H)- 2207 ((1R)-ENDO)-(+)-3- ONE, BROMOCAMPHOR, 98% 12568 (+)-4-CHOLESTEN-3-ONE, 98% 4804 ((1S)-(ENDO,ANTI))-(-)-3- 3774 (+)-5,6-O-CYCLOHEXYLIDENE-L- BROMOCAMPHOR-8- SULFONIC ASCORBIC ACID, 98% ACID, AMMONIUM SALT 11632 (+)-5-BROMO-2'-DEOXYURIDINE, 2208 ((1S)-ENDO)-(-)-3- 97% BROMOCAMPHOR, 98% 11634 (+)-5-FLUORODEOXYURIDINE, 769 ((1S)-ENDO)-(-)-BORNEOL, 99% 98+% 13454 ((2S,3S)-(+)- 11633 (+)-5-IODO-2'-DEOXYURIDINE, 98% BIS(DIPHENYLPHOSPHINO)- 4228 (+)-6-AMINOPENICILLANIC ACID, BUTANE)(N3-ALLYL)PD(II) CL04, 96% 97 8167 (+)-6-METHOXY-ALPHA-METHYL- 10297 ((3- 2- NAPHTHALENEACETIC ACID, DIMETHYLAMINO)PROPYL)TRIPH 98% ENYL- PHOSPHONIUM BROMIDE, 12586 (+)-ANDROSTA-1,4-DIENE-3,17- 99% DIONE, 98% 13458 ((R)-(+)-2,2'- 963 (+)-ARABINOGALACTAN BIS(DIPHENYLPHOSPHINO)-1,1'- -
Common Military List of the European Union
6.4.2016 EN Official Journal of the European Union C 122/1 IV (Notices) NOTICES FROM EUROPEAN UNION INSTITUTIONS, BODIES, OFFICES AND AGENCIES COUNCIL COMMON MILITARY LIST OF THE EUROPEAN UNION adopted by the Council on 14 March 2016 (equipment covered by Council Common Position 2008/944/CFSP defining common rules governing the control of exports of military technology and equipment) (updating and replacing the Common Military List of the European Union adopted by the Council on 9 February 2015 (1)) (CFSP) (2016/C 122/01) Note 1 Terms in ‘quotations’ are defined terms. Refer to ‘Definitions of Terms used in this List’ annexed to this List. Note 2 In some instances chemicals are listed by name and CAS number. The list applies to chemicals of the same structural formula (including hydrates) regardless of name or CAS number. CAS numbers are shown to assist in identifying a particular chemical or mixture, irrespective of nomenclature. CAS numbers cannot be used as unique identifiers because some forms of the listed chemical have different CAS numbers, and mixtures containing a listed chemical may also have different CAS numbers. ML1 Smooth-bore weapons with a calibre of less than 20 mm, other arms and automatic weapons with a calibre of 12,7 mm (calibre 0,50 inches) or less and accessories, as follows, and specially designed components therefor: Note ML1. does not apply to: a. Firearms specially designed for dummy ammunition and which are incapable of discharging a projectile; b. Firearms specially designed to launch tethered projectiles having no high explosive charge or communi cations link, to a range of less than or equal to 500 m; c. -
War Gases .Pdf
yh&% .*i From the collection of the m Prejinger h v Jjibrary San Francisco, California 2007 THE WAR GASES WAR GASES Their Identification and Decontamination BY MORRIS B. JACOBS, Ph.D. Food, Drug and Insecticide Admin. U. S. Dept. of Agr. 1927 Chemist Department of Health, City of New York, 1928. Formerly, Lt. U. S. Chemical Warfare Service Reserve INTERSCIENCE PUBLISHERS, INC. NEW YORK, N. Y.-1942 Copyright, 1942, by INTERSCIENCE PUBLISHERS, INC. 215 Fourth Avenue, New York, N. Y. Printed in U. S. A. by WAVERLY PRESS, BALTIMORE, MD. PREFACE Relatively little has been written in the United States of America on the subject of passive defense, or as we would put it, civilian defense against poison gas. One of the very first steps in defense of this nature is a system for the detection, the sampling and the identification of the chemical war- fare agents, and the decontamination of areas and materials polluted by them. It is the aim of this book to present these subjects so that the informa- tion given will be useful to the gas identification officer, the war gas chemist, the decontamination officer, and the health officer. While this book was written primarily for the aforementioned officers, Chapters I, II, III, part of IV and VII should prove of value to the air raid warden and, in general, to all persons dealing with the above mentioned phases of gas defense. It is written so that it can be used for the training of gas identifi- cation officers, as a manual by chemists and decontamination officers, and as a source of information on the analytical chemistry of the war gases. -
Christian Gloor Journal Club Group Meeting 16 01 2014 .01.2014
Christian Gloor Journal Club Group Meeting 16.01 . 2014 Definitions • Chemical Weapons (CW): − Toxic chemicals and their precursors, except where intended for purposes not prohibited under the convention, as long as the types and quantities are consistent with such purposes − Munitions and devices, specially designed to cause death or other harm • Purposes not prohibited under the convention − Industrial, agricultural, research, medicinal, pharmaceutical or other peaceful purposes − Protective purposes, namely against chemical weapons OPCW Convention on the prohibition of the development, production, stockpiling and use of chemical weapons and on their destruction, Version 2013 Classes of chemical warfare agents y Harassing agents O Cl Cl CN CN Chloracetophenone (CN) Ortho-chlorobenzylidene malononitrile (CS) OH H N Br O O Benzyl bromide Capsaicin (OC) H Cl N As As Cl Diphenylchloroarsine (DA) Adamsite (DM) Classes of chemical warfare agents y Incapacitating agents y Choking agents y Blood agents hdhydrogen cyanide (AC); AAirsine (SA); cyanogen chlor ide (CK) Classes of chemical warfare agents y Blister agents Cl Cl N S As Cl Cl Cl Cl Cl Cl Tris(2-chloroethyl)amine (HN3) Bis(2-chloroethyl) sulfide (HD) 2-Chlorovinyldichloroarsine (L) S S S Cl Cl O Cl Cl S Bis(2-chloroethylthioethyl) ether (T) 1,2-Bis(2-chloroethylthio) ethane (Q) Symptoms of blister agents Classes of chemical warfare agents y Nerve agents Mode of action of nerve agents Antidotes for nerve agents N O O OH Atropin Cl H N O N H Cl N N O O Obidoxim chloride Antidotes y For blister agents A mixture of bleaching powder with 35% active chlorine, molecular sieve, magnesium oxide and silica. -
Rocket Solid Propellant Alternative Based on Ammonium Dinitramide
Rocket Solid Propellant Alternative Based on Ammonium Dinitramide Grigore CICAN*,1, Alexandru-Daniel MITRACHE1 *Corresponding author 1“POLITEHNICA” University of Bucharest, Faculty of Aerospace Engineering, Gh. Polizu Street 1-5, 011061, Bucharest, Romania, [email protected]*, [email protected] DOI: 10.13111/2066-8201.2017.9.1.2 Received: 20 December 2016/ Accepted: 02 February 2017/ Published: March 2017 © Copyright 2017, INCAS. This is an open access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/) International Conference of Aerospace Sciences “AEROSPATIAL 2016” 26 - 27 October 2016, Bucharest, Romania, (held at INCAS, B-dul Iuliu Maniu 220, sector 6) Section 4 – Materials and Structures Abstract: Due to the continuous run for a green environment the current article proposes a new type of solid propellant based on the fairly new synthesized oxidizer, ammonium dinitramide (ADN). Apart of having a higher specific impulse than the worldwide renowned oxidizer, ammonium perchlorate, ADN has the advantage, of leaving behind only nitrogen, oxygen and water after decomposing at high temperatures and therefore totally avoiding the formation of hydrogen chloride fumes. Based on the oxidizer to fuel ratios of the current formulations of the major rocket solid booster (e.g. Space Shuttle’s SRB, Ariane 5’s SRB) which comprises mass variations of ammonium perchlorate oxidizer (70-75%), atomized aluminum powder (10-18%) and polybutadiene binder (12-20%) a new solid propellant was formulated. As previously stated, the new propellant formula and its variations use ADN as oxidizer and erythritol tetranitrate as fuel, keeping the same polybutadiene as binder. -
Scientific Advisory Board
OPCW Scientific Advisory Board Eleventh Session SAB-11/1 11 – 13 February 2008 13 February 2008 Original: ENGLISH REPORT OF THE ELEVENTH SESSION OF THE SCIENTIFIC ADVISORY BOARD 1. AGENDA ITEM ONE – Opening of the Session The Scientific Advisory Board (SAB) met for its Eleventh Session from 11 to 13 February 2008 at the OPCW headquarters in The Hague, the Netherlands. The Session was opened by the Vice-Chairperson of the SAB, Mahdi Balali-Mood. The meeting was chaired by Philip Coleman of South Africa, and Mahdi Balali-Mood of the Islamic Republic of Iran served as Vice-Chairperson. A list of participants appears as Annex 1 to this report. 2. AGENDA ITEM TWO – Adoption of the agenda 2.1 The SAB adopted the following agenda for its Eleventh Session: 1. Opening of the Session 2. Adoption of the agenda 3. Tour de table to introduce new SAB Members 4. Election of the Chairperson and the Vice-Chairperson of the SAB1 5. Welcome address by the Director-General 6. Overview on developments at the OPCW since the last session of the SAB 7. Establishment of a drafting committee 8. Work of the temporary working groups: (a) Consideration of the report of the second meeting of the sampling-and-analysis temporary working group; 1 In accordance with paragraph 1.1 of the rules of procedure for the SAB and the temporary working groups of scientific experts (EC-XIII/DG.2, dated 20 October 1998) CS-2008-5438(E) distributed 28/02/2008 *CS-2008-5438.E* SAB-11/1 page 2 (b) Status report by the Industry Verification Branch on the implementation of sampling and analysis for Article VI inspections; (c) Presentation by the OPCW Laboratory; (d) Update on education and outreach; and (e) Update on the formation of the temporary working group on advances in science and technology and their potential impact on the implementation of the Convention: (i) composition of the group; and (ii) its terms of reference 9. -
United States Patent (19) 11 4,362,884 Arkles (45) Dec
United States Patent (19) 11 4,362,884 Arkles (45) Dec. 7, 1982 (54) SILACROWN ETHERS, METHOD OF MAKING SAME, AND USE AS OTHER PUBLICATIONS PHASE-TRANSFER CATALYSTS C. J. Pederson, J. Am. Chem. Soc., 89, 7017, (1967). R. Kieble, C. Burkhard, J. Am. Chem. Soc., 69, 2689, (75) Inventor: Barry C. Arkles, Oreland, Pa. (1947). (73) Assignee: Petrarch Systems, Inc., Levittown, Primary Examiner-Paul F. Shaver Pa. Attorney, Agent, or Firm-Seidel, Gonda, Goldhammer & Panitch 21) Appl. No.: 323,629 57 ABSTRACT 22 Filed: Nov. 23, 1981 Organosilicon compounds referred to as silacrown ethers or "silacrowns' are of the general formula: (51) Int. Cl............................. C07F 7/08; C07F 7/18 52) U.S. C. .................................... 556/446; 260/464; 560/236; 570/143; 570/145; 570/191; 570/196; 570/197; 570/261 58 Field of Search ......................................... 556/446 where R1 and R2 are organic radicals or hydrogen and 56 References Cited n is an integer between 4 and 10 inclusive. Silacrown U.S. PATENT DOCUMENTS ethers are prepared by reacting polyethylene glycol 3,078,293 2/1963 Ender .................................. 556/446 with substituted silanes under conditions promoting 3,475,478 10/1969 Simmler ..... 556/446X cyclization over polymerization. Silacrown ethers may 3,505,380 4/1970 Berger ................................. 556/446 be employed as phase-transfer catalysts in solution or 3,539,610 1 1/1970 Berger ............................ 536/446X immobilized on siliceous supports. 3,987,061 10/1976 Pedersen ......................... 556/446X 4,098,808 7/1978 Wolfers et al. ..................... 556/446 12 Claims, No Drawings 4,362,884 1 2 SILACROWNETHERS, METHOD OF MAKING DETAILED DESCRIPTION OF THE SAME, AND USE AS PHASE-TRANSFER INVENTION CATALYSTS Silacrowns exhibit complexation properties remark 5 ably similar to crown ethers. -
Preparation of 2-Phenylcyclohexanone and Substituted 2-Arylcyclohenanones
THE PREPARATION OP 2-PHENYLCYCL0HEXAN0NE AND SUBSTITUTED 2-ARYLCYCL0HENAN0NES i . by J RICHARD GRANT HIS KEY A. B., Kansas State Teachers College, Emporia, 1951 A THESIS submitted in partial fulfillment of the requirements for the degree MASTER OP SCIENCE Department of Chemistry KANSAS STATE COLLEGE OF AGRICULTURE AND APPLIED SCIENCE 1953 ii QJUtt A- ViW3» c.cl table op contents I introduction 1 purpose of the investigation 16 results of the investigation ,16 Isolation and Identification of the Intermediate Chlorohydrins 16 Comparison of the Rearrangement of the Cis- and Trans - Chlorohydrins 28 Preparation of Some New 2-Arylcyclohexanones 31 EXPERIMENTAL , . 43 Isolation and Identification of the Intermediate Chlorohydrins 43 Rearrangement of the Cis and Trans Chlorohydrins to 2-Phenylcyclohenanone 49 Preparation of Some New 2-Arylcyclohexanones 51 ACKNOWLEDGMENT 63 BIBLIOGRAPHY 64 INTRODUCTION In recent years both partial syntheses and total syntheses of natural products have become increasingly important. The total synthesis of these products is very desirable since total synthesis of a compound affords a method by which final, con- clusive proof of its structure may be obtained. In addition, the total synthesis might prove economically feasible. For these reasons many workers have attempted to totally synthesize various natural products and their analogs. One of the outstanding examples of the synthesis of a rel- atively complex natural product was that of the female sex hor- mone, equilinln (II), by Bachmann, Cole, and Wilds (1) in 1959- 1940. The last portion of this synthesis utilized the cyclic ketone, 7-methoxy-l-keto-l ,2,5,4 tetrahydro phenanthrene (I) as a key Intermediate.