DOCSLIB.ORG

Arc-Uio Governwent of Inbia Atomic Energy Commission

Total Page：16

File Type：pdf, Size：1020Kb

Download full-text PDF Read full-text
Arc-Uio Governwent of Inbia Atomic Energy Commission •.A.R.C.-UIO 8 v, : '"•' X ' •••--• GOVERNWENT OF INBIA ATOMIC ENERGY COMMISSION METHYLAMINE-HYDROOEN EXCHANdE., PART III. PHYSICOCHEMICAL PROPBRTIBS OF AMIDE-AMINE SOLUTIONS K. S.-:niv»»« »»d S..M. Dtve Heavy Wttw Division BHABHA ATOMIC RESEARCH CENTRE BOMBAV,. INDIA 1983 1.4.1.C.-1180 mortnu. mmomMr cdKxsani at of #iMliM K. MdiM mmt Ml* tor* mi iwM»«t CMMPCT 1112| wit JtflMfl •JtOtlOtS MUTMUUt XDtDKC KOttMS nuntiin Mtiratct nidnizc conuotvntt MMDOCiHot OMKUBMtA AB3TR10T Different p&jrtiooeheaicsl properties of potassiua nethylaaide/niethylaMine solutions' have been complied and reviewed* Vhesi properties will b« quite useful in design calculations for plants based on amine-hydrogen exchange for the production of heavy miter* METFTYLAMINE-HYDROGEW EXdHANGE. PART III. JHYSICOOHEUIGAL PROPERTIES OP AMIDE-AMINE . by K. Srinivaaa and S.M. Dave 1, INTRODUCTION Deuterium exchange between liquid monomethylamine and gaseous hydrogen, catalysed by potassium raethylaraide is emerging as an attractive alternative to the well known ammonia-hydrogen exchange process. The recent studies' * ' indicate that the process has come to a stage where its commercial exploitation ia imminent. The amlne-hydrogen exchange has many favourable features, such aa lower vapour pressures^' , higher exchange rates^'^' and larger separation factors*°*'*°' as compared to the ammonia-hydrogen system and all these advantages lead to considerable lowering of capital and energy costs for heavy v/ater production. Eventh.ough the above mentioned parameters are quite favourable, the process chemistry for this exchange is quite complex and could give rise to some formidable problems. In order to assess the feasibility of this process, it is, therefore, absolutely essential that physical properties and chemical behaviour of the aaine/ amide solutions should be precisely known or predloted for different axperimental conditions* Unfortunately rery meagre information about amine-amide system is available in the published literature. This report attempts to collect necessary and pertinent infornation about this system from various scattered sources and present it in more systematic and usable foxn. (2) PREPARATION OV POTASSIUM METHYMHIEE . ' • Potassium methylamide is most conveniently prepared by the reaction of raonomethylamine with potassium metal''* ', The roaotion is catalysed by traces of transition metal compounds like ferrous chloride or ferrio oxide. The amine rauat be purified from ammonia, moisture and other impuritiea before use. Hie process involves the dissolution of potassium metal in methylamine before the amide formation reaction.' Potassium metal dissolves in methylamine even at -78 0 giving a deep blue solution which becomes pale yellow with the formation of the amide. The yellow colour is more intense at higher temperatures though the amide solution is almoat colourless at -*78 0» '^ie reaction is aaeomi'anied by the evolution of hydrogen. K + CH5lffl2 —• CHg-NHK + %R2 , (1) The evolution of hydrogen is an indication that the reaction is in progress. Hie dissolution of potassium and its subsequent reaction are much slower than in ammonia. The rate of reaction is negligible below -GO 0. !Ehe preparation of potassium methylamide is conveniently carried out at about -6 0. , Even then.it requires several hours for completion. The reaction should not be carried out at higher temperature as this will favour the decomposition of the amide. After preparation the (3) amide solution should be stored below -10*0 to minimise thermal decomposition. In view of the extremely reactive nature of the potassium methylamide the amide solution : . should be handled using vacuum,line and dry box techniques in argon atmosphere* Potassium methylamide can also be obtained by treating methyleonine with potassium hydride' '• In yet another methodv ', the amide has been prepared by adding methylamine to a solution of potassium amide' in liquid ammonia. Frescott and Sanford*": have patented a process for the removal of impurities from potassium raethylaiaide. the method involves converting the KHHOH* into KHHg by reaoting with ammonia and regeneration of KNHOH, by reaction between potassium amide and methylamine. The amides of other alkali metals with other aliphatic amines can be obtained by similar methods. PROPERTIES 0? AIIIPE/AMINE SOIUIIONS Potassium methyIsmids is a white crystalline solid with a relatively high melting point. It reacts vigorously with oxygen, oarbon dioxide, water and aloohdls . It reacts explosively with air and oan ignite spontaneously* Solutions of the amide in methyliaine are also extremely, sensitive to air and moisture. The amide may be safely destroyed by reacting it with «iyl alcohol • Potassium methylamide/methylamine system is similar to (4) potassium amide/ammonia system in many respects* However, some differences are .expected since there is a high degree of association due to the low dieleotrio constant of methylamine and the high negative oharge density on the • nitrogen. • 3.1 Solubility of Amide in Aminea Potassium methylamide exhibits an inverse solubility in methylamine, i.e. its solubility decreases with increasing temperature, so that the amide is precipitated at higher temperatures* The solubility has been measured by Hayashitorai, Ishige and Otto^ ' between -78 and +4O#O. The solubility is 39 £ 3 g' K/Kg amine at -78°C and decreases to about 26 g K/Kg aoine at +40°C. This is surprising* particularly since the solubility of potassium amide in ammonia increases considerably with increasing temperature. This indicates that the dissolution of potassium methylamide has a negative enthalphy change which has been roughly estimated to be of the order of -0.5 Kcal/mole. Table 1 gives the effebt of temperature on the solubility of potassium methylamide in methylamine. The solubility of potassium ethylamide in ethylamine is relatively high and the system ia similar to the. potassium aaide/ammonia system with the solubility increasing markedly with temperature. She solubility at -40*0 is about 90 g K/Kg amine and at .^78*0 it ia at least 25 g K/Kg aaine. (5) 3«2 Viscosity • No data are available on the visoosity of potassium methylaraide solutions in methylamine. However, the viscosity of methylamine is known for different tempe- ratures and is given in Table 2* • 3.3 ftleotrioal Conductivity Symon and Bonnet*1 *' have described' an apparatus for conductivity measurements on potassium methylamide/ methylamine solutions over the temperature range -55 to 425°C. The eleotrode system based on the recommen- dations of Nichol and Puoss* *' consisted of a vertically mounted pair of concentric platinum cylinders. Temperature control and measurement was better than +0.02o0. Equi- valent oonductanoe values (A) were calculated from resistance data applying correction for the specific conductance of the solvent. The data obtained by them are believed to be accurate within A plot of A &t constant temperature against the square root of the amide concentration is reproduced in Fig. 1. The dependence of A on temperature for three different concentrations is shown in Fig. 2. A distinct maximum was observed in each case at about ~30°C. 3*4 Dissociation of Amides Potassium methylamide dissolved in methylamine, dissociates Into free ions as shown below : + KHIICHj =?=* K + ~NHCH3 ....'(2) The dissociation constant was reported to be 3 x 10"*^ mol I" (6) at -90°0 and 4 x 10"7 mol IT1 at -62°C by Rochard^9'16*. Subsequently Symona and Bonnet* "•' found a value of 6.5 x 10~7 mol I."1 at -33.4°C. Since methylamine has a fairly low dieleotrio constant (about 9.4 at 25°G) concentrated solutions of potassium methylamide are expected to consist of a Eixture of free ions, ion pai.rof triple ions and larger ion aggregates. Symons and Bonnet' ^' have made a detailed study of the effect of temperature on the dissociation constant of potassium methyl«roide from conductance measurements made between -55°C and 25°0. These data are reproduced In Table 3. The dissociation constant Kj decreased from 9.4 x 10~7 mol IT1 at -55°0 to 6.3 x 10"8 mol I,"1 at 25°C. The heat of dissociation has been calculated to be -26 kJ mol~ above -15°C. It decreases gradually at progressively lower temperatures. This has been attributed to a change in the nature of the ion pair structures. 3.5 Association of Amides Halliday and Bindner have estimated from kinetic studies, the percentages of the monomer present in potassium methylnmide/methylaininc solutions of different concentrations at different temperatures. These values are given in Table 4. These calculations predict that at 0°C potassium methylaraide should be pre«ent almost entirely as a monomer over a wide concentration range. This is reported to be in agreement with the degree of association calculated from vapour pressure measurements on IMAAlA solutlona' ''. , 4.;- REAO'l'IOHS Off AMIDES . '/ ' ' ','.'. Potassium taethylamide dissolved in methylanine is a strong i base and is highly reactive* It reacts with air and with water so violently that special techniques and apparatus are required for handling the system. Some of the reactions with the impurities usually encountered in the process are described below. 4.1 Reaction with water Potassium methylamide as well as its solution in raethylaraine reacts vigorously with water to give potassium hydroxide and methylamine. - . CRyiHK + H20 —* CHjNEg + KOH .... (3) Potasoiiun hydroxide being insoluble in raethylamine can be removed by filtration in inert atmosphere. When v:ater is in excess the amide is completely decomposed. Amide solutions can be conveniently determined from the quantity of potassium hydroxide formed. 4.2 Reaction v/ith oxygen The reaction of potassium methylamide with oxygen yields potassium dimethylfonnamidine (PBIPA). The reaction is oomplex and is believed to involve several steps. CHjHlIK + 02 -^ KON, KOH, CHjNCH - ITOHj .*.. (4) •':•" K (8) 4*3 Reaction with Carbon monoxide and Carbon dioxide Potassium methylamide, like Potassium amide, reacts with Carbon dioxide and Carbon monoxide forming Potassium jr-methyl oartumate and Potassium N-tnethyl foiwamide , respe ctively. 0H3NHK + C02 —* CHjNHCOOK .... (5) 0 CH,HHK + CO * oL^K .
Load more

Recommended publications
  • Safety Data Sheet
    SAFETY DATA SHEET Revision Date 27-February-2020 Revision Number 2 1. Identification Product Name Potassium hydride, 30% w/w in mineral oil Cat No. : L13266 Synonyms No information available Recommended Use Laboratory chemicals. Uses advised against Food, drug, pesticide or biocidal product use. Details of the supplier of the safety data sheet Company Importer/Distributor Manufacturer Fisher Scientific Alfa Aesar 112 Colonnade Road, Thermo Fisher Scientific Chemicals, Inc. Ottawa, ON K2E 7L6, 30 Bond Street, Ward Hill, MA 01835-8099 Canada Tel: 800-343-0660 Fax: 800-322-4757 Tel: 1-800-234-7437 Email: [email protected] www.alfa.com Emergency Telephone Number During normal business hours (Monday-Friday, 8am-7pm EST), call (800) 343-0660. After normal business hours, call Carechem 24 at (800) 579-7421. 2. Hazard(s) identification Classification WHMIS 2015 Classification Classified as hazardous under the Hazardous Products Regulations (SOR/2015-17) Substances/mixtures which, in contact with water, emit Category 1 flammable gases Skin Corrosion/Irritation Category 1 B Serious Eye Damage/Eye Irritation Category 1 Specific target organ toxicity (single exposure) Category 3 Target Organs - Respiratory system. Aspiration Toxicity Category 1 Physical Hazards Not Otherwise Classified Category 1 Reacts violently with water Label Elements Signal Word Danger Hazard Statements In contact with water releases flammable gases which may ignite spontaneously ______________________________________________________________________________________________ Page 1 / 7 Potassium hydride, 30% w/w in mineral oil Revision Date 27-February-2020 ______________________________________________________________________________________________ May be fatal if swallowed and enters airways Causes severe skin burns and eye damage May cause respiratory irritation Reacts violently with water Precautionary Statements Manufacturer Alfa Aesar Thermo Fisher Scientific Chemicals, Inc.
    [Show full text]
  • Page 1 of 26 RSC Advances
    RSC Advances This is an Accepted Manuscript, which has been through the Royal Society of Chemistry peer review process and has been accepted for publication. Accepted Manuscripts are published online shortly after acceptance, before technical editing, formatting and proof reading. Using this free service, authors can make their results available to the community, in citable form, before we publish the edited article. This Accepted Manuscript will be replaced by the edited, formatted and paginated article as soon as this is available. You can find more information about Accepted Manuscripts in the Information for Authors. Please note that technical editing may introduce minor changes to the text and/or graphics, which may alter content. The journal’s standard Terms & Conditions and the Ethical guidelines still apply. In no event shall the Royal Society of Chemistry be held responsible for any errors or omissions in this Accepted Manuscript or any consequences arising from the use of any information it contains. www.rsc.org/advances Page 1 of 26 RSC Advances The ternary amide KLi 3(NH 2)4: an important intermediate in the potassium compounds-added Li –N–H systems Bao-Xia Dong, Liang Song, Jun Ge, Yun-Lei Teng*, Shi-Yang Zhang College of Chemistry and Chemical Engineering, Yangzhou University, Yangzhou, 225002, P. R. China. In this paper, the KH-added LiH–NH 3, KH-added LiH–LiNH 2, KH-added LiNH 2, and KNH 2-added LiNH 2 systems were systematically investigated. It was found that the ternary amide KLi 3(NH 2)4 was an important intermediate that was inclined to be formed in the dehydrogenation and hydrogenation processes of the potassium compounds-added Li–N–H system.
    [Show full text]
  • Richards2019.Pdf
    This thesis has been submitted in fulfilment of the requirements for a postgraduate degree (e.g. PhD, MPhil, DClinPsychol) at the University of Edinburgh. Please note the following terms and conditions of use: This work is protected by copyright and other intellectual property rights, which are retained by the thesis author, unless otherwise stated. A copy can be downloaded for personal non-commercial research or study, without prior permission or charge. This thesis cannot be reproduced or quoted extensively from without first obtaining permission in writing from the author. The content must not be changed in any way or sold commercially in any format or medium without the formal permission of the author. When referring to this work, full bibliographic details including the author, title, awarding institution and date of the thesis must be given. Exploring Metal-base Catalysis in Indole C2 Selective Mannich and Alkylnitrile Conjugate Addition Reactions Jonathan Richards A thesis submitted for the degree of Doctor of Philosophy The University of Edinburgh 2018 Declaration I, Jonathan Richards, hereby declare that, except where reference has been to other sources that the work contained within this thesis is my original work as part of my PhD degree program. This program of study was commenced August 2014. The thesis has been composed by myself and has not been submitted, in whole or in part, towards any other degree, diploma or qualification. Signed: Date: Acknowledgements I would like to thank Alan Steven and the rest of the Raw group at Astra Zeneca for the welcome atmosphere and great guidance during my time at Macclesfield and for funding the research.
    [Show full text]
  • Chemical Chemical Hazard and Compatibility Information
    Chemical Chemical Hazard and Compatibility Information Acetic Acid HAZARDS & STORAGE: Corrosive and combustible liquid. Serious health hazard. Reacts with oxidizing and alkali materials. Keep above freezing point (62 degrees F) to avoid rupture of carboys and glass containers.. INCOMPATIBILITIES: 2-amino-ethanol, Acetaldehyde, Acetic anhydride, Acids, Alcohol, Amines, 2-Amino-ethanol, Ammonia, Ammonium nitrate, 5-Azidotetrazole, Bases, Bromine pentafluoride, Caustics (strong), Chlorosulfonic acid, Chromic Acid, Chromium trioxide, Chlorine trifluoride, Ethylene imine, Ethylene glycol, Ethylene diamine, Hydrogen cyanide, Hydrogen peroxide, Hydrogen sulfide, Hydroxyl compounds, Ketones, Nitric Acid, Oleum, Oxidizers (strong), P(OCN)3, Perchloric acid, Permanganates, Peroxides, Phenols, Phosphorus isocyanate, Phosphorus trichloride, Potassium hydroxide, Potassium permanganate, Potassium-tert-butoxide, Sodium hydroxide, Sodium peroxide, Sulfuric acid, n-Xylene. Acetone HAZARDS & STORAGE: Store in a cool, dry, well ventilated place. INCOMPATIBILITIES: Acids, Bromine trifluoride, Bromine, Bromoform, Carbon, Chloroform, Chromium oxide, Chromium trioxide, Chromyl chloride, Dioxygen difluoride, Fluorine oxide, Hydrogen peroxide, 2-Methyl-1,2-butadiene, NaOBr, Nitric acid, Nitrosyl chloride, Nitrosyl perchlorate, Nitryl perchlorate, NOCl, Oxidizing materials, Permonosulfuric acid, Peroxomonosulfuric acid, Potassium-tert-butoxide, Sulfur dichloride, Sulfuric acid, thio-Diglycol, Thiotrithiazyl perchlorate, Trichloromelamine, 2,4,6-Trichloro-1,3,5-triazine
    [Show full text]
  • Prohibited and Restricted Chemical List
    School Emergency Response Plan and Management Guide Prohibited and Restricted Chemical List PROHIBITED AND RESTRICTED CHEMICAL LIST Introduction After incidents of laboratory chemical contamination at several schools, DCPS, The American Association for the Advancement of Science (AAAS) and DC Fire and Emergency Management Services developed an aggressive program for chemical control to eliminate student and staff exposure to potential hazardous chemicals. Based upon this program, all principals are required to conduct a complete yearly inventory of all chemicals located at each school building to identify for the removal and disposal of any prohibited/banned chemicals. Prohibited chemicals are those that pose an inherent, immediate, and potentially life- threatening risk, injury, or impairment due to toxicity or other chemical properties to students, staff, or other occupants of the school. These chemicals are prohibited from use and/or storage at the school, and the school is prohibited from purchasing or accepting donations of such chemicals. Restricted chemicals are chemicals that are restricted by use and/or quantities. If restricted chemicals are present at the school, each storage location must be addressed in the school's written emergency plan. Also, plan maps must clearly denote the storage locations of these chemicals. Restricted chemicals—demonstration use only are a subclass in the Restricted chemicals list that are limited to instructor demonstration. Students may not participate in handling or preparation of restricted chemicals as part of a demonstration. If Restricted chemicals—demonstration use only are present at the school, each storage location must be addressed in the school's written emergency plan. Section 7: Appendices – October 2009 37 School Emergency Response Plan and Management Guide Prohibited and Restricted Chemical List Following is a table of chemicals that are Prohibited—banned, Restricted—academic curriculum use, and Restricted—demonstration use only.
    [Show full text]
  • Peroxides and Peroxide- Forming Compounds
    FEATURE Peroxides and peroxide- forming compounds By Donald E. Clark Bretherick5 included a discussion of nated. However, concentrated hydro- organic peroxide5 in a chapter on gen peroxide (Ͼ30%), in contact with norganic and organic peroxides, highly reactive and unstable com- ordinary combustible materials (e.g., because of their exceptional reac- pounds and used “oxygen balance” to fabric, oil, wood, or some resins) Itivity and oxidative potential are predict the stability of individual com- poses significant fire or explosion haz- widely used in research laboratories. pounds and to assess the hazard po- ards. Peroxides of alkali metals are not This review is intended to serve as a tential of an oxidative reaction. Jack- particularly shock sensitive, but can 6 guide to the hazards and safety issues son et al. addressed the use of decompose slowly in the presence of associated with the laboratory use, peroxidizable chemicals in the re- moisture and may react violently with handling, and storage of inorganic and search laboratory and published rec- a variety of substances, including wa- organic peroxy-compounds and per- ommendations for maximum storage ter. Thus, the standard iodide test for oxide-forming compounds. time for common peroxide-forming peroxides must not be used with these The relatively weak oxygen-oxygen laboratory solvents. Several solvents, water-reactive compounds.1 linkage (bond-dissociation energy of (e.g., diethyl ether) commonly used in Inorganic peroxides are used as ox- 20 to 50 kcal moleϪ1) is the character- the laboratory can form explosive re- idizing agents for digestion of organic istic structure of organic and inor- action products through a relatively samples and in the synthesis of or- ganic peroxide molecules, and is the slow oxidation process in the pres- ganic peroxides.
    [Show full text]
  • Chapter 9 Hydrogen
    Chapter 9 Hydrogen Diborane, B2 H6• is the simplest member of a large class of compounds, the electron-deficient boron hydrid Like all boron hydrides, it has a positive standard free energy of formation, and so cannot be prepared direct from boron and hydrogen. The bridge B-H bonds are longer and weaker than the tenninal B-H bonds (13: vs. 1.19 A). 89.1 Reactions of hydrogen compounds? (a) Ca(s) + H2Cg) ~ CaH2Cs). This is the reaction of an active s-me: with hydrogen, which is the way that saline metal hydrides are prepared. (b) NH3(g) + BF)(g) ~ H)N-BF)(g). This is the reaction of a Lewis base and a Lewis acid. The product I Lewis acid-base complex. (c) LiOH(s) + H2(g) ~ NR. Although dihydrogen can behave as an oxidant (e.g., with Li to form LiH) or reductant (e.g., with O2 to form H20), it does not behave as a Br0nsted or Lewis acid or base. It does not r with strong bases, like LiOH, or with strong acids. 89.2 A procedure for making Et3MeSn? A possible procedure is as follows: ~ 2Et)SnH + 2Na 2Na+Et3Sn- + H2 Ja'Et3Sn- + CH3Br ~ Et3MeSn + NaBr 9.1 Where does Hydrogen fit in the periodic chart? (a) Hydrogen in group 1? Hydrogen has one vale electron like the group 1 metals and is stable as W, especially in aqueous media. The other group 1 m have one valence electron and are quite stable as ~ cations in solution and in the solid state as simple 1 salts.
    [Show full text]
  • Hydrogen Ab/Desorption of Lih-KH Composite and Ammonia System Kiyotaka Goshome1,*1, Hiroki Miyaoka2, Hikaru Yamamoto3,*2, Takayuki Ichikawa4,*3 and Yoshitsugu Kojima1
    Materials Transactions, Vol. 57, No. 7 (2016) pp. 1215 to 1219 ©2016 The Japan Institute of Metals and Materials Hydrogen Ab/Desorption of LiH-KH Composite and Ammonia System Kiyotaka Goshome1,*1, Hiroki Miyaoka2, Hikaru Yamamoto3,*2, Takayuki Ichikawa4,*3 and Yoshitsugu Kojima1 1Institute for Advanced Materials Research, Hiroshima University, Higashi-Hiroshima 739–8530, Japan 2Institute for Sustainable Sciences and Development, Hiroshima University, Higashi-Hiroshima 739–8530, Japan 3Graduate School of Advanced Sciences of Matter, Hiroshima University, Higashi-Hiroshima 739–8530, Japan 4Graduate School of Integrated Arts and Sciences, Hiroshima University, Higashi-Hiroshima 739–8521, Japan Lithium hydride-Potassium hydride (LiH-KH) composite prepared by ball-milling is focused in order to modify the kinetic properties of the reaction between LiH and gaseous ammonia (NH3). The LiH-NH3 system is recognized as one of the most promising hydrogen storage system because it generates hydrogen at room temperature by ammonolysis reaction, is regenerated below 300°C, and possesses more than 8.0 mass% hydrogen capacity. From the experimental results, it is conrmed that the hydrogen generation from the reaction between NH3 and the LiH-KH composite shows much higher reaction rate than that of the simple summation of each component, which can be recognized as a synergetic effect. Then, double-cation metal amide (MNH2) phases such as LiK(NH2)2, which are not assigned to any amides reported before, are formed as the reaction product. Moreover, it is conrmed that hydrogenation of the generated amide can proceed to form LiH-KH compos- ite and NH3. [doi:10.2320/matertrans.M2016071] (Received February 26, 2016; Accepted April 26, 2016; Published May 27, 2016) Keywords: ammonia, metal hydrides, double-cation amide, ammonolysis 1.
    [Show full text]
  • Valparaiso University Laboratory Safety Manual
    VALPARAISO UNIVERSITY LABORATORY SAFETY MANUAL 36 Table of Contents INTRODUCTION 3 RESPONSIBILITIES 3 INFORMATION AND TRAINING 5 Training 5 Medical Program 6 Emergency Procedures 7 STANDARD OPERATING PROCEDURES 9 Personal Safety and Responsibility 9 Personal Protective Equipment (PPE) 11 Chemical Specific Procedures 12 Compressed Gases and Cryogenic Liquids 14 Exposure Determination 17 LABORATORY CONTROLS 17 Chemical Fume Hoods 17 General Laboratory Ventilation 18 Fire Alarm System 19 Emergency Eyewashes and Safety Showers 19 CHEMICAL PROCUREMENT AND STORAGE PROCEDURES 19 Chemical Procurement 19 Chemical Storage 20 Peroxide Testing 21 Hazard Identification 22 ENVIRONMENTAL AND WASTE MANAGEMENT 24 Protection of the Air 24 Protection of the Water 24 Hazardous Waste Management 25 APPENDIX Appendix 1: Schedule of Events 29 36 Appendix 2: Laboratory Chemical Hood Preventative Maintenance 30 Appendix 3: Peroxide Testing Process 33 INTRODUCTION Valparaiso University is dedicated to protecting the health and safety of its laboratory users through compliance with applicable local, state, and federal regulations. The Occupational Safety and Health Administration (OSHA) established 29 CFR 1910.1450, Occupational Exposure to Hazardous Chemicals in Laboratories, on Jan. 31, 1990, to provide guidelines for the safe use of chemicals in laboratories. This standard applies in locations where laboratory use of hazardous chemicals occurs and there is a risk of exposure. Laboratory use of hazardous chemicals entails the handling or use of chemicals in containers that can easily and safely be manipulated by one person or where multiple chemicals or chemical procedures are used. The purpose of this Laboratory Safety Manual is to provide all laboratory workers and students a plan to avoid unnecessary chemical exposures and to address basic standard operating procedures (emergency procedures, chemical procurement, maintenance, etc.) that are used at Valparaiso University and to provide the necessary framework for compliance with the OSHA Lab Standard.
    [Show full text]
  • Chemical Compatibility Storage Group
    CHEMICAL SEGREGATION Chemicals are to be segregated into 11 different categories depending on the compatibility of that chemical with other chemicals The Storage Groups are as follows: Group A – Compatible Organic Acids Group B – Compatible Pyrophoric & Water Reactive Materials Group C – Compatible Inorganic Bases Group D – Compatible Organic Acids Group E – Compatible Oxidizers including Peroxides Group F– Compatible Inorganic Acids not including Oxidizers or Combustible Group G – Not Intrinsically Reactive or Flammable or Combustible Group J* – Poison Compressed Gases Group K* – Compatible Explosive or other highly Unstable Material Group L – Non-Reactive Flammable and Combustible, including solvents Group X* – Incompatible with ALL other storage groups The following is a list of chemicals and their compatibility storage codes. This is not a complete list of chemicals, but is provided to give examples of each storage group: Storage Group A 94‐75‐7 2,4‐D (2,4‐Dichlorophenoxyacetic acid) 94‐82‐6 2,4‐DB 609-99-4 3,5-Dinitrosalicylic acid 64‐19‐7 Acetic acid (Flammable liquid @ 102°F avoid alcohols, Amines, ox agents see SDS) 631-61-8 Acetic acid, Ammonium salt (Ammonium acetate) 108-24-7 Acetic anhydride (Flammable liquid @102°F avoid alcohols see SDS) 79‐10‐7 Acrylic acid Peroxide Former 65‐85‐0 Benzoic acid 98‐07‐7 Benzotrichloride 98‐88‐4 Benzoyl chloride 107-92-6 Butyric Acid 115‐28‐6 Chlorendic acid 79‐11‐8 Chloroacetic acid 627‐11‐2 Chloroethyl chloroformate 77‐92‐9 Citric acid 5949-29-1 Citric acid monohydrate 57-00-1 Creatine 20624-25-3
    [Show full text]
  • 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28
    Appendix B Classification of common chemicals by chemical band 1 1 EXHIBIT 1 2 CHEMICAL CLASSIFICATION LIST 3 4 1. Pyrophoric Chemicals 5 1.1. Aluminum alkyls: R3A1, R2A1C1, RA1C12 6 Examples: Et3A1, Et2A1C1, EtA.1111C12, Me3A1, Diethylethoxyaluminium 7 1.2. Grignard Reagents: RMgX (R=alkyl, aryl, vinyl X=halogen) 8 1.3. Lithium Reagents: RLi (R 7 alkyls, aryls, vinyls) 9 Examples: Butyllithium, Isobutylthhium, sec-Butyllithium, tert-Butyllithium, 10 Ethyllithium, Isopropyllithium, Methyllithium, (Trimethylsilyl)methyllithium, 11 Phenyllithiurn, 2-Thienyllithium, Vinyllithium, Lithium acetylide ethylenediamine 12 complex, Lithium (trimethylsilyl)acetylide, Lithium phenylacetylide 13 1.4. Zinc Alkyl Reagents: RZnX, R2Zn 14 Examples: Et2Zn 15 1.5. Metal carbonyls: Lithium carbonyl, Nickel tetracarbonyl, Dicobalt octacarbonyl 16 1.6. Metal powders (finely divided): Bismuth, Calcium, Cobalt, Hafnium, Iron, 17 Magnesium, Titanium, Uranium, Zinc, Zirconium 18 1.7. Low Valent Metals: Titanium dichloride 19 1.8. Metal hydrides: Potassium Hydride, Sodium hydride, Lithium Aluminum Hydride, 20 Diethylaluminium hydride, Diisobutylaluminum hydride 21 1.9. Nonmetal hydrides: Arsine, Boranes, Diethylarsine, diethylphosphine, Germane, 22 Phosphine, phenylphosphine, Silane, Methanetellurol (CH3TeH) 23 1.10. Non-metal alkyls: R3B, R3P, R3As; Tributylphosphine, Dichloro(methyl)silane 24 1.11. Used hydrogenation catalysts: Raney nickel, Palladium, Platinum 25 1.12. Activated Copper fuel cell catalysts, e.g. Cu/ZnO/A1203 26 1.13. Finely Divided Sulfides:
    [Show full text]
  • Potassium Hydride, 20-25% Wt.% Dispersion in Mineral Oil
    Material Safety Data Sheet Potassium Hydride, 20-25% wt.% Dispersion in Mineral Oil MSDS# 00046 Section 1 - Chemical Product and Company Identification MSDS Name: Potassium Hydride, 20-25% wt.% Dispersion in Mineral Oil Catalog Numbers: AC201710000, AC201710250, AC201711000 Synonyms: None. Acros Organics BVBA Company Identification: Janssen Pharmaceuticalaan 3a 2440 Geel, Belgium Acros Organics Company Identification: (USA) One Reagent Lane Fair Lawn, NJ 07410 For information in the US, call: 800-ACROS-01 For information in Europe, call: +32 14 57 52 11 Emergency Number, Europe: +32 14 57 52 99 Emergency Number US: 201-796-7100 CHEMTREC Phone Number, US: 800-424-9300 CHEMTREC Phone Number, Europe: 703-527-3887 Section 2 - Composition, Information on Ingredients ---------------------------------------- Risk Phrases: 11 14/15 34 CAS#: 7693-26-7 Chemical Name: POTASSIUM HYDRIDE %: 20 - 25 EINECS#: 231-704-8 Hazard Symbols: F C ---------------------------------------- ---------------------------------------- Risk Phrases: CAS#: 8042-47-5 Chemical Name: MINERAL OIL %: 75 - 80 EINECS#: 232-455-8 Hazard Symbols: ---------------------------------------- Text for R-phrases: see Section 16 Hazard Symbols: F C Risk Phrases: 11 14/15 34 Section 3 - Hazards Identification EMERGENCY OVERVIEW Danger! Water-reactive. Highly flammable. May cause central nervous system depression. Causes eye and skin burns. Causes digestive and respiratory tract burns. Dangerous when wet. Reacts violently with water liberating highly flammable gases. Target Organs: Central nervous system, eyes, skin, mucous membranes. Potential Health Effects Eye: Causes eye burns. Skin: Causes skin burns. May cause cyanosis of the extremities. Ingestion: Causes gastrointestinal tract burns. Ingestion of large amounts may cause CNS depression. Causes chemical burns to the respiratory tract.
    [Show full text]