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FS/2018 ORGANIC CHEMISTRY I LAB CHEM 226 (2219) Instructor
FS/2018 ORGANIC CHEMISTRY I LAB CHEM 226 (2219) Instructor: Terry Bone 120-B Schrenk Hall [email protected] 341-4820 http://www.mst.edu/~tbone 9:00-10:00, Tu-Th, or by appt. Cynthia Bolon 213 Schrenk Hall [email protected] 341-4439 OBJECTIVES: Course objectives are to develop facility with performing laboratory techniques involving the handling of organic chemicals safely and the keeping of proper records of experiments conducted in the laboratory. Crystallization, distillation, extraction and chromatography are emphasized as separation and purification techniques. Melting points, boiling points, and refractive indices are used routinely as measures of purity. Safe handling of chemicals and proper disposal of waste products are priority goals in this course. To help in attaining such goals, the first week of the semester is devoted to SAFETY in the chemistry laboratory. For the remainder of the semester, most of the experiments are conducted on a micro scale. BOOKS: 1. 100 pg. set Organic Chemistry Laboratory Notebook 2. “Organic Chemistry Laboratory Laboratory Techniques, 2nd ed”. Available as free pdf download at https://open.umn.edu/opentextbooks/BookDetail.aspx?bookId=369 3. “Microscale Techniques for the Organic Laboratory, 2nd ed”, (MTOL), Mayo, Pike, Butcher and Trumper, John Wiley & Sons, Inc.,2001 (on reserve at library circulation desk-currently out of print but available on Amazon) 4. “Right to Know pocket guide for School & University Employees”, Genium Publishing Corp., 1990. (optional) (#1 can be purchased from the book store) LAB SYLLABUS: Originally prepared by Prof. S. B. Hanna, modified by D. E. Hoiness, T.Bone. GENERAL GUIDELINES SAFETY Goggles must be worn at all times in the lab. -
EWRE Lab Regulations
Department of Civil & Environmental Engineering University of Massachusetts College of Engineering University of Massachusetts September 2012 CONTENTS UNIVERSITY OF MASSACHUSETTS ......................................................................................................................... 1 CONTENTS ...................................................................................................................................................................... 2 A. LABORATORY SAFETY AND SECURITY ........................................................................................................... 1 1. GENERAL RULES .......................................................................................................................................................... 1 2. EMERGENCY ................................................................................................................................................................ 2 3. DISPOSAL OF CHEMICALS ............................................................................................................................................ 2 a. What chemical wastes are hazardous or non-hazardous? ...................................................................................... 2 b. Disposal of hazardous wastes ................................................................................................................................. 2 4. FUME HOODS .............................................................................................................................................................. -
Multigram Chromatography-Free Synthesis of Octa (Ethylene Glycol) P
ORGANIC CHEMISTRY FRONTIERS View Article Online METHOD View Journal | View Issue Multigram chromatography-free synthesis of octa(ethylene glycol) p-toluenesulfonate† Cite this: Org. Chem. Front., 2016, 3, 1524 Adam M. Wawro,a Takahiro Muraoka,b,c Maho Katob and Kazushi Kinbara*b Here we report a detailed synthetic procedure for monodisperse octa(ethylene glycol) p-toluenesulfonate, Received 27th July 2016, a member of the heterobifunctional oligo(ethylene glycol) derivatives family. The method offers Accepted 3rd September 2016 completely chromatography-free workup and purification, resulting in higher yields and a lower cost than DOI: 10.1039/c6qo00398b any of the alternative strategies. We also introduce several upgrades, simplifying the method even more, rsc.li/frontiers-organic and discuss the chromatography-free design limitations. Introduction building blocks of functional compounds. Although tradition- ally PEGs have been produced by polymerization, yielding stat- Creative Commons Attribution-NonCommercial 3.0 Unported Licence. Poly(ethylene glycol)s (PEGs) are frequently used in chemistry, istically distributed mixtures of individual polymer molecules, most notably for protein cross-linking and modification, the recent demand for more uniform PEGs has stimulated surface functionalization, and as flexible and hydrophilic studies on well-defined, single-molecule polymers. These PEGs, known as ‘discrete’, ‘unimolecular’ or ‘monodisperse’, consist of a single chemical species with a specific molecular a Institute of Multidisciplinary Research for Advanced Materials, Tohoku University, weight. Monodisperse PEGs are obtained by classical step- 2-1-1 Katahira, Aoba-ku, Sendai 980-8577, Japan bSchool of Life Science and Technology, Tokyo Institute of Technology, by-step chemical synthesis, usually from inexpensive short 4259 Nagatsuta-cho, Midori-ku, Yokohama 226-8501, Japan. -
Volumetric Labware Volumetric Labware
Volumetric Labware Volumetric Labware Volumetric Glassware NABL Certificate Please see list of Accreditation Bodies Worldwide from Page 148-151 38 Volumetric Labware In ASTM standards cylinders are now calibrated "to deliver" (TD), which has been recently introduce in Cylinder section. 39 Volumetric Labware BATCH CERTIFICATE Volumetric flasks comes with a batch certificate in which mean value, standard deviation is incorporated along with batch number like which signifies the month 01 and 10 is the year 01.10 This comes in a pack of 1 and comes along with the flask in the box you can also download it from www.glasscolabs.com and by scanning the QR Code from the label of the box. QR CODES ! Scan For Certicates Now On Cartons Of All Glassco Wares! Use your Smartphone to scan the QR Code on the box labels … Just select the Certicate you wish to see… Conformity… Calibration … (Individual or Batch) INDIVIDUAL CERTIFICATE These flasks comes with a certificate on which individual serial number, mean value, standard deviation and measured uncertainty is given along with the batch number and serial number like 01.10 (Month and year of manufacturing) 505 (serial number) 01.10 5 0 5 This comes in a pack of one and each flask is having a certificate with it in the box you can also download it from www.glasscolabs.com and by scanning the QR Code from the label of the box. USP Glassware All the volumetric glassware or measuring instruments to be used in laboratories which are under surveillance of US authorities such as Food and Drug Administration (FDA), have a mandatory requirement to use products which adhere to standards set by US PHARMACOPEIA. -
Reducible Sulfur in Paper and Paperboard (Revision of T 406 Om-08) (No Changes from Draft 2)
NOTICE: This is a DRAFT of a TAPPI Standard in ballot. Although available for public viewing, it is still under TAPPI’s copyright and may not be reproduced or distributed without permission of TAPPI. This draft is NOT a currently published TAPPI Standard. WI 120802.02 T 406 DRAFT NO. 3 DATE April 30, 2013 WORKING GROUP CHAIRMAN James C. Abbott SUBJECT CATEGORY Chemical Properties RELATED METHODS See “Additional Information” CAUTION: This Test Method may include safety precautions which are believed to be appropriate at the time of publication of the method. The intent of these is to alert the user of the method to safety issues related to such use. The user is responsible for determining that the safety precautions are complete and are appropriate to their use of the method, and for ensuring that suitable safety practices have not changed since publication of the method. This method may require the use, disposal, or both, of chemicals which may present serious health hazards to humans. Procedures for the handling of such substances are set forth on Material Safety Data Sheets which must be developed by all manufacturers and importers of potentially hazardous chemicals and maintained by all distributors of potentially hazardous chemicals. Prior to the use of this method, the user must determine whether any of the chemicals to be used or disposed of are potentially hazardous and, if so, must follow strictly the procedures specified by both the manufacturer, as well as local, state, and federal authorities for safe use and disposal of these chemicals. Reducible sulfur in paper and paperboard (Revision of T 406 om-08) (no changes from Draft 2) 1. -
Sulfur Dioxide
Corn Sugar (crude & refined) Analysis F-54-1 SULFUR DIOXIDE PRINCIPLE Sulfur dioxide is released by boiling an acidic sample solution, and it is removed by sweeping with a stream of nitrogen. The gas stream is passed through dilute hydrogen peroxide solution where sulfur dioxide is oxidized to sulfuric acid. The acid is titrated with standard alkali. (Note 1) SCOPE The method applies to crude and refined sugars (Note 2) and, with minor modification, to most liquid and solid samples even in the presence of other volatile compounds. SPECIAL APPARATUS 1. The FDA modified "Monier-Williams" apparatus (Figure 1) is available from Fisher Scientific, 91/92 Cat. No. K513800 (Kontes 513800), Pittsburgh, PA, and affiliates worldwide. It or some of its parts are also available from other laboratory supply houses. (Note 3) 2. Heating mantle, for a 1000 mL boiling flask, controlled by a variable transformer. 3. Flow controlling valve, with flow indicator, capable of controlling nitrogen gas flow to 200 mL/min. 4. Refrigerated, circulating bath capable of maintaining flow through condenser at 5-10 °C (Note 4) 5. Vortex mixer 6. Buret, class A, 10 mL 7. Pipet bulb Analytical Methods of the Member Companies of the Corn Refiners Association, Inc. Accepted 11-13-61 Revised 4-9-91 Corn Sugar (crude & refined) Analysis F-54-2 SULFUR DIOXIDE ⎯ continued REAGENTS 1. Hydrogen Peroxide Solution, 3%: Dilute 10 mL of C.P. neutral 30% hydrogen peroxide (H2O2) with purified water to 100 mL. Prepare daily. 2. Sodium Hydroxide Solution, 0.01 N: Dilute 10 mL of 0.100 N NaOH solution to 100 mL. -
Azoniaspiro Salts: Towards Bridging the Gap Between Room-Temperature Ionic Liquids and Molten Salts
Electronic Supplementary Material (ESI) for Physical Chemistry Chemical Physics. This journal is © the Owner Societies 2016 Azoniaspiro salts: towards bridging the gap between room-temperature ionic liquids and molten salts Matthew T. Clough,a,b Karolin Geyer,c Patricia A. Hunt,*a Alastair J. S. McIntosh,a Rebecca Rowe,a Tom Welton*a and Andrew J. P. Whitea a Department of Chemistry, Imperial College London, London, UK, SW7 2AZ, United Kingdom b Max-Planck-Institut für Kohlenforschung, 45470 Mülheim-an-der-Ruhr, Germany c BASF SE, Ludwigshafen, Germany * Corresponding Authors: [email protected] [email protected] Electronic Supplementary Information 1. General laboratory procedures 2 2. Synthesis of ionic compounds 2 3. TGA procedures 8 4. TGA-MS procedures 9 5. TGA-GCMS procedures 9 6. X-Ray Crystallography procedures and data 10 7. Computational methods 12 8. Ion pair conformers and transition state structures 13 1 1. General laboratory procedures All reactions requiring an inert atmosphere were performed under a blanket of nitrogen gas, which was dried through a column of phosphorus pentoxide. All commercially acquired chemicals were obtained from Sigma- Aldrich or Tokyo Chemical Industry, and were used without further purification unless otherwise stated. Anhydrous solvents were dried through an HPLC column on an Innovative Technology Inc. solvent purification system. NMR spectra were recorded on Bruker Avance-400 (1H NMR (400 MHz), 13C (100 MHz), 19F (376 MHz)) NMR spectrometers. Chemical shifts are reported in ppm (relative to the DMSO-d6 residual peak). IR spectra were recorded on a Perkin Elmer spectrum 100 FTIR using an ATR inset with a diamond crystal. -
Laboratory Manual
International Program UAM-Boston University Laboratory Manual Organic Chemistry I 2013-2014 Departamento de Química Orgánica Ernesto Brunet Romero Ana María Martín Castro Ramón Gómez Arrayás Laboratory Manual Table of Contents ............................................................................... 1 Introduction ............................................................................... 2 Prelab preparation ............................................................................... 2 Notebook ............................................................................. 3 Safety .............................................................................. 3 Laboratory Practices and Safety Rules ............................................................. 4 Accidents and injuries ........................................................................... 5 Fires ............................................................................. 5 Chemical Wastes ............................................................................. 6 Cleaning Responsibilities ............................................................................. 6 Lab cleanliness ............................................................................. 6 Laboratory Equipment ............................................................................. 7 Proper use of glassware ............................................................................. 8 Some techniques in lab experiments Heating, cooling and stirring ............................................................................ -
Isolation and Characterization of a Natural Product: Caffeine
Cerritos Community College Organic Chemistry 211 Laboratory Isolation and Characterization of a Natural Product: Caffeine. O O CH3 N H HN – H3C N O N N O N N P OH H2N N O O N N N N O H3C OH purine 2'-deoxyguanosine caffeine 5'-phosphate In this experiment, the techniques of solid-liquid extraction and liquid-liquid extraction will be used to isolate caffeine from tealeaves. A new purification technique, sublimation, will be used to perform the final purification. Caffeine is a member of the class of natural products called alkaloids, which contain nitrogen. Other members of this class include morphine, mescaline, and strychnine. The strong biological activity of these compounds has led to their thorough investigation by many different disciplines. Caffeine possesses the oxidized skeleton of purine, a relative of which can be found as a constituent of DNA (see above). Caffeine is found in many plants with coffee and tea being the most familiar. A cup of coffee or tea provides a 25- to 100-mg “Dose” of caffeine, which stimulates the central nervous system in a widely exploited manner. From the preceding, it is not surprising that caffeine is soluble in hot water, but it is also soluble in dichloromethane, allowing the following extractive protocol to isolate it. This two-step extractive isolation assures that ionic species remain in the aqueous layer while taking advantage of the swelling that water causes in the tea leaves. Simply extracting the tealeaves with dichloromethane directly is ineffective. The sodium carbonate added to the water during the “steeping” stage is to insure that the caffeine and organic acids are deprotonated. -
5-Solution Unknown
College Prep Chemistry Lab Manual Written, compiled, edited by Brian Cox and Dan Albritton Thanks to Daniel Knowles, Eddie Taylor, Dylan Muzny, Cammie Wickham Table of Contents Reference Laboratory Safety Guidelines i, ii Lab Experiments Pages Expt #1: 5-Solution Unknown 1-2 Data Analysis: How does the Mass of Pennies Change with Age? 3-5 Expt #2: Relationship between Mass of Reactants to Mass of Products 6-13 Expt #3: Distillation: Separation of two liquids 14-17 Expt #4: Observing the Chemistry of Iron(II) and Iron(III) 18-19 Expt #5: An Activity Series of Metals (Single Replacement Rxns) 20-21 Expt #6: Precipitation Reactions (Double Replacement Rxns) 22-23 Expt #7: Recording Measurements with Correct Sig Figures and 24-26 Uncertainty Expt #8: Mole Concept – How many atoms or molecules are present? 27-30 Expt #9: Empirical Formula of a Hydrate 31-33 Expt #10: Density of Twizzler Sticks 34-35 Expt #11: A Taste of Molarity 36 Expt #12: Preparing Molar Solutions 37- 38 Expt #13: Demos to investigate concept of limiting reactant and optimal 39-42 ratio Expt #14: Determination of Percent Yield – How efficient is your reaction? 43-46 Expt #15: Determination of Universal Gas Constant 47-51 Expt #16: Emission Spectrum and Quantum Leaps 52-55 Expt #17: Beer’s Law: Determining Molar Concentration by Absorbance 56-60 Spectroscopy Expt #18: Relationship between Type of Chemical Bonds and Electrical 61-64 Conductivity Expt #19: Molecular Models (Drawing in 3-D) 65-67 Expt #20: Polar and Non-Polar Molecules in an Electric Field 68-69 Expt #21: Molecular -
Chemistry 1009 Lab Manual University of Louisiana at Monroe
Chemistry 1009 Lab Manual University of Louisiana at Monroe Department of Chemistry 2010 Version 2.0 Contents Lab Session 1: Laboratory Safety Rules and Check In .................................................. 1 Fire, Injury, Spills and Cleanliness .............................................................................. 2 Desk Assignment Sheet (Chemistry 1009) .................................................................. 4 Commonly Used Equipment (not in the desk drawer)................................................. 5 Lab Session 2, Experiment 1: Introductory Exercises ................................................... 10 Report Form 1 .............................................................................................................. 17 Lab Session 3, Experiment 2: Oxygen ........................................................................... 18 Report Form 2 .............................................................................................................. 21 Lab Session 4, Experiment 3: Preparation of Sodium Chloride .................................... 22 Report Form 3 .............................................................................................................. 25 Lab Session 5, Experiment 4: Law of Definite Proportions .......................................... 26 Report Form 4 ........................................................................................................... 30 Lab Session 6, Experiment 5: Hydrogen and the Activity Series of Metals ................. -
PIRANHA SOLUTION CLEANING Rev
Section 4: Laboratory SOPs – Procedure Form Title: PIRANHA SOLUTION CLEANING Rev. Date: 08/06/18 Prepared By: P.I.: Prior Approval: This procedure is considered hazardous enough that prior approval is needed from the Principal Investigator: Y N Involves Use of Particularly Hazardous Substance (PHS)? Y N Carcinogen Reproductive Toxin High Acute Toxicity Does this procedure require medical surveillance? Y N Does this require use of a fit-tested respirator? Y N A Piranha solution is a mix of concentrated sulfuric acid with hydrogen peroxide, and generally used to Bremoverief Description organic residues of Procedure from substrates. (100 wordsSee prep or below: less): 1. Transfer sulfuric acid to a large, clean Pyrex glass beaker. (NO PLASTIC CONTAINERS) 2. Slowly add 1 part 30% hydrogen peroxide to 3 parts concentrated sulfuric acid inside a chemical fume hood using PPE described below. Use a dropping funnel to add hydrogen peroxide to sulfuric acid with continuous stirring. (use a Teflon coated stir bar) 3. Slowly place clean microscope slides and coverslips into the solution for 1 hour using long tongs to avoid skin exposure. 4. Remove slides/coverslips with tongs and sonicate in milliQ water for 10 minutes. 5. Allow piranha solution to cool to room temperature in an open container. 6. Transfer cooled solution to a clean and dry vented waste container for disposal. Safety Notes: All piranha manipulations shall be conducted inside a properly functional chemical fume hood. Keep all containers in secondary containment at all times. Prepare solution immediately before use. Avoid all contact between piranha solution and organic materials.