Glovebox General Use
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Dalton Transactions
Dalton Transactions View Article Online PAPER View Journal | View Issue The role of neutral Rh(PONOP)H, free NMe2H, boronium and ammonium salts in the dehydro- Cite this: Dalton Trans., 2019, 48, 14724 coupling of dimethylamine-borane using the 2 + cationic pincer [Rh(PONOP)(η -H2)] catalyst†‡ E. Anastasia K. Spearing-Ewyn,a Nicholas A. Beattie,b Annie L. Colebatch, a Antonio J. Martinez-Martinez, a Andrew Docker,a Timothy M. Boyd,a Gregg Baillie,b Rachel Reed,b Stuart A. Macgregor *b and Andrew S. Weller *a 1 F 3 The σ-amine-borane pincer complex [Rh(PONOP)(η -H3B·NMe3)][BAr 4][2, PONOP = κ -NC5H3-2,6- t 2 F (OP Bu2)2] is prepared by addition of H3B·NMe3 to the dihydrogen precursor [Rh(PONOP)(η -H2)][BAr 4], 1 F 1. In a similar way the related H3B·NMe2H complex [Rh(PONOP)(η -H3B·NMe2H)][BAr 4], 3, can be made in situ, but this undergoes dehydrocoupling to reform 1 and give the aminoborane dimer [H2BNMe2]2. Creative Commons Attribution 3.0 Unported Licence. NMR studies on this system reveal an intermediate neutral hydride forms, Rh(PONOP)H, 4, that has been prepared independently. 1 is a competent catalyst (2 mol%, ∼30 min) for the dehydrocoupling of H3B·Me2H. Kinetic, mechanistic and computational studies point to the role of NMe2H in both forming the neutral hydride, via deprotonation of a σ-amine-borane complex and formation of aminoborane, and Received 17th August 2019, closing the catalytic cycle by reprotonation of the hydride by the thus-formed dimethyl ammonium Accepted 3rd September 2019 + + [NMe2H2] . -
Elements of a Glovebox Glove Integrity Program
RESEARCH ARTICLE Elements of a Glovebox Glove Integrity Program Programmatic operations at the Los Alamos National Laboratory Plutonium Facility involve working with various amounts of plutonium and other highly toxic, alpha-emitting materials. The spread of radiological contamination on surfaces and airborne contamination and excursions of contaminants into the operator’s breathing zone are prevented through the use of a variety of gloveboxes. The glovebox gloves are the weakest part of this engineering control. As a matter of good business practice, a team of glovebox experts from Los Alamos National Laboratory has been assembled to proactively investigate processes and procedures that minimize unplanned openings in the glovebox gloves, i.e., breaches and failures. Working together, they have developed the key elements of an efficient Glovebox Glove Integrity Program (GGIP). In the following report, the consequences of a glove failure or breach are identified, the acceptable risk is clarified, and elements needed to implement an efficient GGIP are discussed. By Michael E. Cournoyer, INTRODUCTION Through an integrated approach, Julio M. Castro, controls have been developed and Michelle B. Lee, Plutonium requires a high degree of implemented that come from input Cindy M. Lawton, confinement and continuous control from glovebox workers, scientists, Young Ho Park, measures in nuclear research labora- health physicists, statisticians, and phy- Roy Lee, tories because of its extremely low sical therapists. Working together, they Stephen Schreiber permissible body burden.1 Methods have developed an efficient Glovebox and equipment must be designed Glove Integrity Program (GGIP). toward the ultimate accomplishment Recent accomplishes of this team have 2–5 Michael E. -
Water Loss from Terrestrial Planets with CO2-Rich Atmospheres
Water loss from terrestrial planets with CO2-rich atmospheres R. D. Wordsworth Department of the Geophysical Sciences, University of Chicago, 60637 IL, USA [email protected] and R. T. Pierrehumbert Department of the Geophysical Sciences, University of Chicago, 60637 IL, USA ABSTRACT Water photolysis and hydrogen loss from the upper atmospheres of terrestrial planets is of fundamental importance to climate evolution but remains poorly understood in general. Here we present a range of calculations we performed to study the dependence of water loss rates from terrestrial planets on a range of atmospheric and external parameters. We show that CO2 can only cause sig- nificant water loss by increasing surface temperatures over a narrow range of conditions, with cooling of the middle and upper atmosphere acting as a bottle- neck on escape in other circumstances. Around G-stars, efficient loss only occurs on planets with intermediate CO2 atmospheric partial pressures (0.1 to 1 bar) that receive a net flux close to the critical runaway greenhouse limit. Because G-star total luminosity increases with time but XUV/UV luminosity decreases, this places strong limits on water loss for planets like Earth. In contrast, for a CO2-rich early Venus, diffusion limits on water loss are only important if clouds caused strong cooling, implying that scenarios where the planet never had surface liquid water are indeed plausible. Around M-stars, water loss is primarily a func- arXiv:1306.3266v2 [astro-ph.EP] 12 Oct 2013 tion of orbital distance, with planets that absorb less flux than ∼ 270 W m−2 (global mean) unlikely to lose more than one Earth ocean of H2O over their lifetimes unless they lose all their atmospheric N2/CO2 early on. -
General Glovebox Rules
Glovebox etiquette in the Lewis group Introduction: The gloveboxes are here to assist you in oxygen and water sensitive chemistry. The following guidelines are given to protect the box atmosphere and longevity and ultimately your chemistry and that of the whole group. If you feel that these guidelines impede your ability to do work, talk about it with the person in charge of the glovebox and they will help assist you in designing a set up that will work for you! Disregarding the guidelines compromises your chemistry as well as everyone elses. Available boxes: *Big Bird – Vac, purchased 2008. Drybox, Ar. Noyes 227B. Use for electrochemistry. O2 < 0.5 ppm *Snuffleupagus – Vac, older than time. Drybox, N2. Noyes 227B. Use for electrochemistry and storage. Absolutely no bad solvents/chemicals with the exception of CH3CN open for <5 minutes at a time. O2 < 1 ppm *Oscar the Grouch – Vac, older than time. Flushbox, N2. Noyes 227B. Alcohol OK. Electrochemistry, set-up, surface chemistry. O2 < 10 ppm *Elmo – Vac, purchased 2008. Drybox, N2. BI 032. Electrochemistry and chemical synthesis. O2 < 0.5 ppm *Count von Count – Mbraun, less old than time. Drybox, N2. BI 032. Don, Tony, electrochemistry and set up. O2 < 1 ppm *Cookie Monster – Vac, eh? As old as time?. Flushbox, N2. BI 023. Alcohol OK. Electrochemistry, set-up, surface chemistry. Connected to XPS. O2 < 10 ppm Note: Contact Box Czar before using a new box – even if you are trained on the old box. If nothing else, so they can keep track of who is using what and include you on important info for that box. -
Cold Traps out of Glass Or Stainless Steel for the Vacuum Technology
Cold traps out of glass or stainless steel for the vacuum technology KGW-ISOTHERM Karlsruher Glastechnisches Werk 76185 Karlsruhe Gablonzerstraße 6 Tel:0721/ 95897-0 Fax: 0721 / 95897-77 Email: [email protected] Internet: www.kgw-isotherm.com A 16 Cold traps: construction, operation and principles Cold traps are used in conjunction with vacuum pumps to collect condensation produced from humidity or solvents and these cold traps can be used for many different tasks. The most common application is collecting condensation produced from humidity or solvents from rotating discs, vacuum pumps or high vacuum systems that use‘s oil diffusion or turbo-molecular pumps. In this case a common coolant such as liquid nitrogen (LN2) or dry-ice (CO2) with acetone is normally used. Another application is the production of condensation from specific substances at a constant, predefined temperature. This can be realised by using a coolant at a constant, predefined temperature, a thermostat or a Kaltgas system. Cold traps can be manufactured out of glass or metal. The use of glass is advantageous in the chemical sector and when producing condensation from solvents, due to its resistance to chemicals. All glass cold traps listed in this catalogue are produced solely from borosilicate glass 3.3, in compliance with DIN/ISO (DURAN made by Schott). The mechanical design takes into account the wall thickness for use under vacuum. Material - glass All the glassware produced by KGW - ISOTHERM are made of borosilicat glass 3.3 DIN/ISO 3585. The glass has the following characteristics: Chemical characteristics hydrolytic resistance : according to DIN-ISO 719 (98°C) acid resistance : according to DIN-ISO 1776 alkaline resistance : according to ISO 695-A2 Physical characteristics linear expansion factor : 3,3 x 10-6 1/K (at 20°C-300°C) density : 2,23 g/cm3 specific thermal capacity : 910 J/kg K transformation temperature : 525 °C Admissible Operation Conditions for cold traps made of glass Temperature range -200°C to +200 °C Pressure range standard vacuum to atm. -
Medical Management of Persons Internally Contaminated with Radionuclides in a Nuclear Or Radiological Emergency
CONTAMINATION EPR-INTERNAL AND RESPONSE PREPAREDNESS EMERGENCY EPR-INTERNAL EPR-INTERNAL CONTAMINATION CONTAMINATION 2018 2018 2018 Medical Management of Persons Internally Contaminated with Radionuclides in a Nuclear or Radiological Emergency Contaminatedin aNuclear with Radionuclides Internally of Persons Management Medical Medical Management of Persons Internally Contaminated with Radionuclides in a Nuclear or Radiological Emergency A Manual for Medical Personnel Jointly sponsored by the Endorsed by AMERICAN SOCIETY FOR RADIATION ONCOLOGY INTERNATIONAL ATOMIC ENERGY AGENCY V I E N N A ISSN 2518–685X @ IAEA SAFETY STANDARDS AND RELATED PUBLICATIONS IAEA SAFETY STANDARDS Under the terms of Article III of its Statute, the IAEA is authorized to establish or adopt standards of safety for protection of health and minimization of danger to life and property, and to provide for the application of these standards. The publications by means of which the IAEA establishes standards are issued in the IAEA Safety Standards Series. This series covers nuclear safety, radiation safety, transport safety and waste safety. The publication categories in the series are Safety Fundamentals, Safety Requirements and Safety Guides. Information on the IAEA’s safety standards programme is available on the IAEA Internet site http://www-ns.iaea.org/standards/ The site provides the texts in English of published and draft safety standards. The texts of safety standards issued in Arabic, Chinese, French, Russian and Spanish, the IAEA Safety Glossary and a status report for safety standards under development are also available. For further information, please contact the IAEA at: Vienna International Centre, PO Box 100, 1400 Vienna, Austria. All users of IAEA safety standards are invited to inform the IAEA of experience in their use (e.g. -
Environmental Health and Safety Vacuum Traps
Environmental Health and Safety Vacuum Traps Always place an appropriate trap between experimental apparatus and the vacuum source. The vacuum trap: • protects the pump, pump oil and piping from the potentially damaging effects of the material; • protects people who must work on the vacuum lines or system, and; • prevents vapors and related odors from being emitted back into the laboratory or system exhaust. Improper trapping can allow vapor to be emitted from the exhaust of the vacuum system, resulting in either reentry into the laboratory and building or potential exposure to maintenance workers. Proper traps are important for both local pumps and building systems. Proper Trapping Techniques To prevent contamination, all lines leading from experimental apparatus to the vacuum source must be equipped with filtration or other trapping as appropriate. • Particulates: use filtration capable of efficiently trapping the particles in the size range being generated. • Biological Material: use a High Efficiency Particulate Air (HEPA) filter. Liquid disinfectant (e.g. bleach or other appropriate material) traps may also be required. • Aqueous or non-volatile liquids: a filter flask at room temperature is adequate to prevent liquids from getting to the vacuum source. • Solvents and other volatile liquids: use a cold trap of sufficient size and cold enough to condense vapors generated, followed by a filter flask capable of collecting fluid that could be aspirated out of the cold trap. • Highly reactive, corrosive or toxic gases: use a sorbent canister or scrubbing device capable of trapping the gas. Environmental Health and Safety 632-6410 January 2010 EHSD0365 (01/10) Page 1 of 2 www.stonybrook.edu/ehs Cold Traps For most volatile liquids, a cold trap using a slush of dry ice and either isopropanol or ethanol is sufficient (to -78 deg. -
Standard Glovebox Workstations
STANDARD GLOVEBOX WORKSTATIONS www.mbraun.com Light Hood *Freezer Flange DN 40 KF Adjustable Shelving Large Antechamber *Analyzers *Small Antechamber Fine Filter Stainless Steel Piping Programmable Logic Controller Glove Ports Gas Purification System Castors for Easy Mobility Vacuum Pump Leveling Feet Foot Switch *LABstar glovebox workstation is pictured with optional features MBRAUN GLOVEBOX WORKSTATION GLOVEBOX MBRAUN Light Hood Touch Screen PLC Controller *Freezer Adjustable Shelving Large Antechamber *Analyzers Flange DN 40 KF Glove Ports *Small Antechamber Stainless Steel Piping Fine Filter Gas Purification System Castors for Easy Mobility Leveling feet Foot Switch Flow Meter *UNIlab glovebox workstation is pictured with optional features Light Hood Color Touch Screen PLC Controller Adjustable Shelving Large Antechamber Glove Ports *Small Antechamber Fine Filter Flange DN 40 KF Gas Purification Single (SP) or Double (DP) Purifier Unit *External Solvent Trap Castors for Easy Mobility Vacuum Pump Foot Switch Leveling Feet *LABmaster SP/DP glovebox workstation is pictured with optional features GLOVEBOX CONFIGURATIONS MAY VARY LABstar Standard Features: • Programmable logic controller • Large main antechamber • Three glovebox sizes available LAB • Vacuum pump • Automatic regenerable H O/O WORKSTATION 2 2 single column inert gas purifier • World-wide operation using standard power supply The LABstar workstation is a ready to operate high • Integrated high vacuum feedthroughs • Stainless steel adjustable shelving quality glovebox system -
LC-1 Stand Alone Glovebox Operation Manual
LC-1 Stand Alone Glovebox Operation Manual Table of Contents 1. System Overview Page 4 2. Installation Instructions Page 5 - 8 2.1 Attach Gloves Page 5 2.2 Glovebox Connections Page 6 - 8 3. Operational Instructions Page 9 - 39 3.1 Purge System Page 9 - 13 3.1.1 Purging without a Purge Valve Page 9 - 10 3.1.2 Purging with a Manual Purge Valve Page 11 - 12 3.1.3 Purging with an Automatic Purge Valve Page 13 3.2 Normal / Circulation Mode Page 14 - 15 3.3 Antechamber Operation Page 16 - 25 3.3.1 Antechamber Door Operation for Systems Without an Page 16 -17 Antechamber 3.3.2 Antechamber Door Operation for Systems With an Page 18 - 21 Antechamber 3.3.2.1 Bringing Items into Glovebox Page 18 - 20 3.3.2.2 Removing Items from Glovebox Page 21 3.3.3 Mini Antechamber Operation Page 22 - 23 3.3.4 Automatic Antechamber Control Page 24 - 25 3.4 Regeneration Mode Page 26 - 27 3.5 Service Mode Page 28 - 32 3.6 Analyzers Page 33 3.7A Manual Solvent Removal System Operation & Maintenance Page 34 - 35 3.7.1A Manual Solvent Removal System Operation Page 34 3.7.2A Manual Solvent Removal System Maintenance Page 35 3.7B Automatic Solvent Removal System Operation Page 36 - 37 3.7.1B Automatic Solvent Removal System Operation Page 36 3.7.2B Automatic Solvent Removal Reactivation Page 37 3.8 Freezer Operation and Maintenance Page 38 - 39 3.8.1 Freezer Operation Page 38 3.8.2 Freezer Maintenance Page 39 3.9 Box Cooling Operation Page 40 2 3.10 Alarm Messages Page 41 - 42 3.11 Window Removal Page 43 3.12 Window Replacement Page 44 3.13 Maintenance Schedule & Recommended Spare Parts Page 45 3 LC-1 Stand Alone Glovebox Operation Manual Section 1: System Overview Antechamber Star Knobs Antechamber Evacuate/Refill Buttons -35°C Freezer Vacuum Gauge Mini Antechamber Window Frame Mini Antechamber Evacuate/Refill Valve Glove Ports PLC Controller Chiller Butyl Gloves Electrical Cabinet Foot Pedals Gas Purification System Power Switch Solvent Removal System Blower Vacuum Filter Pump Column 4 Section 2: Installation Instructions 2.1 Attach Gloves -Place glove onto the glove port. -
Hearing Conservation
Stench Chemicals Stench chemicals are a group of chemicals that exhibit an extremely foul smell. Even though most stench chemicals have little direct impact on the physical health and safety of researchers, use of these chemicals without an odor control plan can have an effect on both the laboratory environment as well as the outside environment. Therefore, it is important that researchers carefully control their use of all stench chemicals in order to minimize the impact on other workers and neighbors. Examples of Stench Compounds A few examples of stench chemicals are: thiols (mercaptans), sulfides, selenides, amines, phosphines, butyric acid and valeric acid. Among the chemicals listed above, thiols, also referred to as mercaptans, are the most commonly used group, and are therefore discussed in further detail below. Thiols (Mercaptans) Thiols are a class of organosulfur compounds characterized by the presence of one or more sulfhydryl (-SH) groups. Since 1937, thiols have been added to natural gas (which is naturally odorless) as an odorant to assist with detecting natural gas leaks. Thiols exhibit a moderate level of toxicity, and their use does not require special safety precautions. Thiols are characterized by their disagreeable odors at parts per million (ppm) concentrations, and have an odor threshold of only 0.011 ppm. Due to their addition to natural gas, the detection of their odor automatically leads to suspicion of natural gas leaks in or near buildings where they are used. Thus, the use of even small quantities of thiols in laboratory experiments without odor control measures in place can cause concern for other building occupants, people passing by outside, or even the occupants of adjacent buildings. -
PDF (4 Chapter 2.Pdf)
-82- Chapter 2 The Synthesis and Reactivity of Group 7 Carbonyl Derivatives Relevant to Synthesis Gas Conversion -83- Abstract Various Group 7 carbonyl complexes have been synthesized. Reduction of these complexes with hydride sources, such as LiHBEt3, led to the formation of formyl species. A more electrophilic carbonyl precursor, [Mn(PPh3)(CO)5][BF4], reacted with transition metal hydrides to form a highly reactive formyl product. Moreover, a diformyl species was obtained when [Re(CO)4(P(C6H4(p-CF3))3)2][BF4] was treated with excess LiHBEt3. The synthesis and reactivity of novel borane-stabilized Group 7 formyl complexes is also presented. The new carbene-like species display remarkable stability compared to the corresponding “naked” formyl complexes. Reactivity differs significantly whether BF3 or B(C6F5)3 binds the formyl oxygen. Unlike other analogs, Mn(CO)3(PPh3)2(CHOB(C6F5)3) is not stable over time and undergoes decomposition to a manganese carbonyl borohydride complex. Cationic Fischer carbenes were prepared by the reaction of the corresponding formyl species with electrophiles trimethylsilyl triflate and methyl triflate. While the siloxycarbene product is highly unstable at room temperature, the methoxy carbene is stable both in solution and in the solid state. Treating the methoxycarbene complexes with a hydride led to the formation of methoxymethyl species. Manganese methoxymethyl complexes are susceptible to SN2-type attack by a hydride to release dimethyl ether and a manganese anion, which presumably proceeds with further reaction with reactive impurities or borane present. Furthermore, subjecting manganese methoxymethyl complexes to an atmosphere of CO led to the formation of acyl products via migratory insertion. -
Standard Operating Procedures Standard Operating Procedures Tolman Laboratory
Tolman Group Standard Operating Procedures Standard Operating Procedures Tolman Laboratory v.7 updated May 2016 The intent of this manual is to inform you, the chemist, of the potential hazards that exist in the laboratory. This is by no means a manual to memorize or a manual of instruction. These procedures are not intended to be exhaustive or to serve as a single method of training. The procedures outlined here are meant as a refresher for those who have already received training by senior lab members. If in doubt of any procedure, please ask someone before carrying out said procedure. Asking for help when in doubt is the responsibility of every lab member. The first time you use all equipment and perform new experimental procedures, you should have someone work with you to teach you and to inform you of potential hazards, and to help prevent accidents. The purpose of this manual is to supplement personal one-on-one training with safety information that will protect you personally, as well as other lab members. It is important to make sure that you minimize your exposure to chemicals and decrease the chances of any accidents. By reviewing (and later referring to) this manual, you can be aware of the potential hazards in the lab and learn careful techniques. It is your responsibility to learn about safety and proper handling of chemicals from the resources available, including your laboratory members, other persons in the department, and the Chemical Hygiene Plan, which can be accessed via the web, from the Safety link on the Chemistry Webpage www.chem.umn.edu, or http://www.chem.umn.edu/services/safety/.