Setting up the laboratory

Many modern procedures which have now become standard methodology in organic chemistry require dry reaction conditions, and often an inert atmosphere. This has had a dramatic effect on the way efficient laboratory facilities are arranged. Not so long ago reactions involving anhydrous, inert conditions were rare and it was expedient to arrange the equipment for such procedures on a one-off basis. However, now that this type of reaction is common place, it makes sense to set up the laboratory in such a way that reactions under inert conditions can be carried out as a matter of routine. This chapter is written with this principle in mind. Much of the equipment introduced here will be discussed in more detail in subsequent chapters. 

The basic furniture provided in organic chemistry laboratories will vary considerably from one establishment to another and clearly any advice given in this chapter will have to be tailored to the facilities available. The ideal layout of the lab is also a very subjective matter and the advice given here is therefore not intended to be taken as gospel, but simply reflects the experiences of the authors from various laboratories in which they have worked. 

When setting up the lab it is usual for some areas of bench space to be set aside for communal apparatus, and other parts to be allocated as individual benches. Clearly, the areas which are assigned as communal bench space will depend on the amount and type of communal equipment which is to be installed. In this chapter some pieces of equipment will be identified as communal and others as part of the individual bench kit, but the classification will vary from one laboratory to another. The distinction will to some extent depend on the type of work being undertaken, but will also depend on the budget and space available. 

Unless alternative office space is provided, it is a good idea to have some desk space in the lab where workers can read and write, away from areas used for chemicals. Desk space may also be required for small computers which are a common feature of the modem organic chemistry lab. Drawers or filing cabinets are useful for the safe storage of spectra and other paperwork, and a blackboard is an invaluable laboratory aid. 

The area which constitutes an individual bench wiU vary considerably from one lab to another. In our view all procedures involving organic chemicals should be carried out in an efficient fume cupboard. This implies that each full-time wo er in an organic chemistry lab permanently requires at least one metre of fume cupboard space. However, in practice it is often the case, particularly in academic labs, that much less fume cupboard space is actually provided, and fume cupboards may be communal. In this chapter the term bench will refer to the space occupied by an individual worker and it wiU be assumed that this space incorporates an adequate area of fume cupboard, where all reactions are carried out. 

---

At present few hospital laboratories use gas chromatographic methods because colorimetric, fluorometric, and other spectro-photometric methods can give data more rapidly, are less expensive, and are often of sufficient accuracy and precision for clinical evaluation of the patient. Radioimmunoassay procedures are available, but these are limited because of availability of the necessary antibodies and a sufficient demand to justify the expense of setting up the laboratory. For versatility and adaptability, many different analyses can be done on a single gas chromatograph. The only requirement is the proper column and choice of operating conditions. Furthermore, the techniques, in many cases, are now automated. The utility of GC coupled with... 

Costas A. Varotsos received his B.Sc. in Physics at Athens University in 1980, and a Ph.D. in Atmospheric Physics in 1984. He was appointed Assistant Professor in 1989 at the Laboratory of Meteorology of the Physics Department of the Athens University, where he also set up the Laboratory of the Middle and Upper Atmosphere. In 1999 he became Associate Professor of the Department of Applied Physics at Athens University. He is Editor of the International Journal of Remote Sensing and Advisor to the Environmental Science Pollution Research journal. He has published more than 300 papers and 20 books in the fields of atmospheric physics, atmospheric chemistry, and global change. 

Joe Chatt and The Fry the were as great a success academically as Sir Wallace Akers, the ICI Director of Research responsible for setting up the laboratory, had hoped for, but people always ask, Did the Company get anything out of it They certainly did not get a mega-invention such as polythene (which had been developed in one of their Divisional labs.). There were certainly near-misses at the Corporate Labs., Steve O Brien found that zirconium tetra(Tr-allyl) was a... 

The preliminary practices for arranging the ritual space also include setting up the laboratory, which is described in chapter 7 of the commentary. 

This textbook was written to teach radioanalytical chemistry in the classroom and support its application in the laboratory. Its emphasis is on the practical aspects of the specialty, notably setting up the laboratory, training its staff, and operating it reliably. The information presented herein, outlined in Section 1.4, is the accumulated product of a century of nuclear chemistry and radiochemistry practice. 

In 1907, she went to Berlin to study under Max Planck, promising her devoted parents that she would return to Vienna in six months at the most. She stayed in Berlin for thirty-one years. In Berlin, Meitner met Otto Flahn, a professor of chemistiy, and took an unpaid position assisting Flahn with his research on the chemistry of radioactive substances. At that time women were not allowed to v ork in the Chemical Institute, and she had to set up her laboratory in a carpenter s workshop outside the Institute. 

The batch experiment had neither incoming fresh media nor any product stream leaving the fermentation vessel. A complete experimental set up with a B. Braun Biostat, is shown in the above laboratory experimental set up. The continuous flow of media requires a feed tank and product reservoir. The batch process has many disadvantages such as substrate and product inhibition, whereas in the continuous process the fresh nutrients may remove any toxic by-product formed. 

The Production Department was not amused, because lower values had been expected. Quality Control was blamed for using an insensitive, unse-lective, and imprecise test, and thereby unnecessarily frightening top management. This outcome had been anticipated, and a better method, namely polarography, was already being set up. The same samples were run, this time in duplicate, with much the same results. A relative confidence interval of 25% was assumed. Because of increased specificity, there were now less doubts as to the amounts of this particular heavy metal that were actually present. To rule out artifacts, the four samples were sent to outside laboratories to do repeat tests with different methods X-ray fluorescence (XRFi °) and inductively coupled plasma spectrometry (ICP). The confidence limits were determined to be 10% resp. 3%. Figure 4.23 summarizes the results. Because each method has its own specificity pattern, and is subject to intrinsic artifacts, a direct statistical comparison cannot be performed without first correcting the apparent concentrations in order to obtain presumably true... 

It is relevant to present here some preliminaries as regards the salt bridge, this being a traditionally used and more convenient way than the porous partitioning medium in setting up a laboratory assemblage of an electrochemical cell. In this premise, attention is focused on the line formulae of the two cells as presented below ... 

Figure 11(A) shows a principle sketch of a SEC set-up. The eluent (solvent) is pumped at a constant flow rate through the system. A small amount of polymer solution (typically 200 pL) is injected manually or with an autosampler. The main part comprises a set of columns (typically 3-4 columns+pre-column) typically packed with microporous styrene-divinylbenzene, porous glass, or silica. In the routine analytical laboratory it is especially useful to have a pre-column in order to collect impurities that might be present in the samples. If many different samples are to be analyzed, it is necessary to check the reliability of the columns frequently to avoid artefacts due to residues from previous samples still held on the column. In order to avoid problems, samples should be purified before they...

CSI began development of its own hydroxylamine production process through laboratory-scale experimentation in 1997. Development continued with the construction of a 10 gal pilot plant, which was operational in early 1998. In July 1998, CSI leased approximately 20,000 square feet in a multiple-tenant building and began to set up the production facility. 

See Nier, "Emergence of Physics," 279. William Thomson set up the first physics laboratory of its kind in Britain at the University of Glasgow. Alexander Wood, The Cavendish Laboratory (Cambridge Cambridge University Press, 1946) 1. 

We now discuss in detail setting up the partial equilibrium model for a particular case. The dissolution of chalcopyrite, CuFeS2, has been studied extensively in the laboratory ( 3,4 5) and we have been interested in it because of its importance in dump leaching. Under dump leaching conditions, two dissolution reactions have been identified for this mineral (3,4 5) ... 

Setting up a laboratory to run crystallization experiments will not require a huge investment of resources for the initial trials. This will allow to carry out the routine crystallization trials on a protein. If you are planning this to become a major portion of your research program, then a more significant investment will become necessary. The basic components required for crystallization are ... 

There are many variations on setting up the inlets to the MUX interface, depending on the needs of the laboratory. In one setup, one pump is used to deliver the flow through a flow splitter and multiple probe injector to four LC columns.The flow from each column is then fed into the MUX interface. In another variation, on-line SPE is coupled with LC. One pump, followed by a flow splitter, and one four-injector autosampler are used to feed samples into four extraction columns. A second pump is used (again with a flow splitter) to run gradients on the four LC columns into the MUX interface. In yet another system, an eight-channel UV MUX system is utilized. ... 

This is the waste coming from the production of more units than demanded. The optimum number of products to be produced must balance the demand, including that in high season periods, the cost of holding the stocks in the warehouse and the cost of setting up the production to produce one lot of the product. In terms of an analytical laboratory, overproduction could be interpreted as any activity that is not necessary for customer service or for adding value to the experience and knowledge of the laboratory. There is no need to analyse too many samples unless we have reasons to do so. Furthermore, there is no need to perform more analyses than necessary. Too many analytical results are a waste. For example, the optimum number of replicates must balance the need for statistical evaluation. 

Boyle first became interested in natural philosophy during the late 1640s, and he was intrigued by the idea of alchemical transmutations from the very first. From the time he set up a laboratory in Stalbridge to the end of his life, the pursuit of the Philosopher s Stone was always one of his preoccupations. Boyle s personal library contained numerous books on alchemy, and a great many manuscripts describing alchemical experiments were found among his papers after his death. 

Mendeleev and Anna had to find a new apartment, because the university provided the one they were living in. When they had moved in, Mendeleev set up a laboratory in one of the rooms. This allowed him to continue to perform experiments and to submit papers to scientific journals. 

---