Working in the Laboratory

Note that rather detailed experimental procedures are given early in the textbook, whereas somewhat less detailed instructions are provided later on. This is because many of the basic laboratory operations will have become familiar to you in time and need not be spelled out. It is hoped that this approach to the design of procedures will decrease your tendency to think that you are essentially following a recipe in a cookbook. Moreover, many of the experimental procedures given in the literature of organic chemistry are relatively brief and require the chemist to fill in the blanks, so it is valuable to gain some initial experience in figuring out some details on your own. 

We ve inserted markers in the form of stars ( ) in many of the experimental procedures in this textbook. These indicate places where the procedure can be interrupted without affecting the final outcome of the experiment. These markers are designed to help you make the most efficient use of your time in the laboratory. For example, you may be able to start a procedure at a point in the period when there is insufficient time to complete it but enough time to be able to work through to the location of a star you can then safely store the reaction mixture and finish the sequence during the next laboratory period. We ve not inserted stars at every possible stopping point but only at those where it is not necessarily obvious that interruption of the procedure will have no effect on the experimental results. Consult your instructor if in doubt about whether a proper stopping point has been reached. 

As noted above, a carefully written notebook and proper safety procedures are important components of an experimental laboratory course. These aspects are discussed further in the following two sections. 

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All glassware should be scrupulously clean and, for most purposes, dry before being employed in preparative work in the laboratory. It is well to develop the habit of cleaning all glass apparatus immediately after use the nature of the dirt will, in general, be known at the time, and, furthermore, the cleaning process becomes more difficult if the dirty apparatus is allowed to stand for any considerable period, particularly if volatile solvents have evaporated in the meantime. 

It is regretted that the size of the volume has rendered the insertion of literature references impossible the Selected Bibliography (A,5) may partly compensate for this omission. Section numbers are now included in the headings of the pages—a feature introduced in response to requests by many readers. The volume comprises virtually at least three books under one cover, viz., experimental technique, preparations, and qualitative organic analysis. It should therefore continue to be of value as a one volume reference work in the laboratory. Students at all levels will find their requirements for laboratory work (excluding quantitative organic analysis) adequately provided for and, furthermore, the writer hopes that the book will be used as a source of information to supplement their theoretical studies. 

Marie Cui ie, working in the laboratory with her husband Pierre. (AP/ A/ide World Photos)... 

Fields of Application for ion-selective electrodes o Routine-analytical work in the laboratory (direct or as end-point indicators application frequency in industry 30%) o Clinical analyzers for Na+, K.+, Ca2+, pH, pC02, etc. o Process analyzers... 

Alexander W. Williamson (1824-1904) was born in London, England, and received his Ph.D. at the University of Giessen in 1846. His ability to work in the laboratory was hampered by a childhood injury that caused the ioss of an arm. From 1849 until 1887, he was professor of chemistry at University College, London. 

You have had opportunities to ask many Why questions already from your work in the laboratory. In fact, there are enough such questions to provide the basis for the rest of the course. Some of the questions that have been raised in your experiments are listed at the end of the chapter. Can you add to this list How many of the questions can you answer now We will find the answers to many of them in our subsequent study. Some may not yet have satisfactory answers. These are the most interesting questions because they point into the future— your future. 

However, the work could not be done without the enthusiastic cooperation of all the people in our department, of which I should particularly mention Dipl. Chem. Chr. Leis and Dipl. Chem. H. Handwerker, who performed most of the experimental work in the laboratory. 

It will be appreciated that the Tables are far from complete, but they do contain most of the common organic compounds which the student is likely to encounter in the course of his work in the laboratory. For compounds which are not listed in the Tables, reference should 1m made to larger treatises. These include ... 

When scientists perform experiments, they make observations, collect and analyze data, and formulate generalizations about the data. When you work in the laboratory, you should record all your data in a laboratory report. An analysis of data is easier if all data are recorded in an organized, logical manner. Tables and graphs are often used for this purpose. 

Early work in the laboratory and in the field soon established the fact that there would be no poison residue factor with this chemical, owing to its rapid decomposition. Within a relatively few hours the chemical broke down into diethyl phosphoric acid... 

Albertus, Frater. The work in the laboratory a paradox. Essentia 2, no. 3 (Fall 1981). rhttp // homepages.ihug.com.au/ panopus/essentia/essentiaii3, htm paradoxl. 

One day, as Carothers worked in the laboratory, poisonous bromine spilled on his face and legs, and bromine gas filled his lungs. It could have been far worse the young man working beside Carothers lost most of his penis. Hospitalized for a week as chunks of flesh fell from his leg, Carothers wondered whether chemistry was worth the struggle. He taught at a major university but had no accident insurance, and his bank balance stood at 1.00. He longed for someone to talk to about literature and philosophy, but his classmates read only science. Laboratory air caused an unpleasant dermatitis on various parts of his body. 

The work which casts the most light on our subject, is, I think, that of the Conia and the Fitjer groups. It appears from several joint papers that the younger man had worked in the laboratory of the elder, and perhaps thus increased his interest in spirans of great beauty1. 

We are grateful to Lisa Lindqvist for helpful comments on the manuscript. R. C. is supported by a CIHR Cancer Consortium Post-doctoral Training Grant Award. Work in the laboratory is supported by grants from the Canadian Institutes of Health Research, National Cancer Institute of Canada, and NIH (CA114475). 

Early natural product research with marine mollusks supported a conclusion that all secondary metabolites of mollusks are diet-derived, which proved to be premature. In fact, the biosynthetic capability of some marine mollusks covers a wide spectrum of chemical classes and substances. Much of this recent insight has resulted from work in the laboratories of the authors of Chapter 3. 

William Fraser was born in Hamilton. He studied at the other of the two local universities, Strathclyde, where he obtained a first class B.Sc. honors degree in 1986 and Ph.D. in 1989 under the direction of Professor Colin J. Suckling and Professor Hamish C. S. Wood. He was awarded a Royal Society European Exchange Postdoctoral Fellowship and worked in the laboratories of Professor Albert Eschenmoser at the ETH, Zurich. In 1991, he took up his present position as lecturer in medicinal chemistry at Aston University, Birmingham. His scientific interests include nucleoside and nucleic acid chemistry, solid-supported, synthesis, and study of base-modified antigene oligonucleotides targeted to DNA. 

That s an attitude you might hold while working in the laboratory. You are NOT going to do anything, or get anything done to you, that will require medical attention. If you do get cut, and the cut is not serious, wash the area with water. If there s serious bleeding, apply direct pressure with a clean, preferably sterile, dressing. For a minor bum, let cold water run over the burned area. For chemical bums to the eyes or skin, flush the area with lots of water. In every case, get to a physician if at all possible. 

SACHEM Inc. of Cleburne, Texas, manufactures various concentrations of tetramethylammo-nium hydroxide (TMAH) solutions to meet customer specifications. To ensure consistent performance, electronic industry requires very narrow concentration specifications for the solutions. In SACHEM s quality control laboratory, standardized acids such as HC1 or H2S04 are used as titrants for the TMAH solutions to check their concentrations. The performance of the assay titration is controlled by daily analysis of internal reference standards (IRSs). If the IRS results are within controlled limits, then the assay results of a product can be reported. If not, the results cannot be reported until the root cause is uncovered and eliminated. Safety glasses and gloves are worn while performing this work in the laboratory. 

Always be watchful and considerate of others working in the laboratory. It is important not to jeopardize their safety or yours. 

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