Download Download PDF. Translate PDF. Key words: Microscale chemistry, laboratory, history of chemistry. Even before that, there Microscale Chemistry workshop at Univer- were some relevant -although isolated- sidad Iberoamericana in Mexico City. Zvi Szafran -one of the founders of the country. In many cases, however, you will find that itwill be necessary to modify given procedures, resulting from the unavailability.
The procedure written in the laboratory notebook should be the exact procedure that was actually followed. Any unusual assemblies of glassware should be sketched. Any numbers entered should have units associated with them. It is usually convenient to number each reaction step. Any observations of chemical or physical change should be noted after the experimental step that produced them. For example, one might write:.
The zinc-mercury amalgam is then added to the reaction mixture, which is gently swirled. The vanadium V solution changes color from yellow to blue at this point.
When the experimental procedure is completed, any calculations made using the data obtained should be clearly performed, with an indication as to where any external numbers came from. Enough information should be provided to allow the next scientist using the notebook to perform another calculation on a new set of data.
Finally, you should sign the entry at the very end, and date the work once again. For a legally binding document, a witness should also sign the work.
These parts include the abstract, introduction, experimental section, data section, discussion, conclusions, acknowledgments, and references. It may be that a shorter version of the laboratory report may be acceptable for a par- ticular course. It is always wise to ask the laboratory instructor as to the proper format. Most scientific reports are written in the passive voice, for example, "The solution was mixed for 10 min" rather than "I mixed the solution for 10 min.
It is found at the beginning of a laboratory report so that an individual can get a quick overview of the experiment and decide if they wish to read any further. The abstract is followed by the introduction, where a brief background as to the technique s used in the experiment is outlined. The theory behind any unusual calculations should be presented in the introduction as well. The intro- duction should not go into great detail about material that is readily found else- where; sources for this information should be listed in the reference section.
The experimental section should begin with a listing of where the chem- icals used were obtained, what the purity was, and any prior purification of the. The manufacturer and model number of all major equipment should also be listed. The manner in which spectra were obtained should be included, for example:. The experimental equipment and glassware should be described, with a diagram provided if necessary. All steps performed in the experimental procedure should be listed in the order that they were performed, in exactlythe manner in which you performed them.
Do not list a step as written in some experimental procedure that was followed unless you actually performed that step in an identical fashion.
The source of the experimental procedure if one exists should be referenced. The data should be compiled into tables, if appropriate. Calculations should be made here percent yield, heat of reactions, etc. The data should be discussed and evaluated, both positively and negatively, in the discussion section. D Proper Citation and Plagiarism Let the data "speak for itself," and evaluate the data fairly,.
A dis- cussion of possible sources of error should be included in this section. The results should be summarized and conclusions drawn in the conclu- sions section. In situations where more than one explanation of the data is possible, all explanations should be presented, compared, and contrasted. Any help that was provided to you over the course of the experiment should be mentioned in the acknowledgment section.
There are two common types of reference to printed work; that for a journal article and that for a book. Journal articles are referenced by listing the authors last name first , the title of the journal usually abbreviated, in italics , the year of publication boldface , the volume number italics , and the page number. For example:. Smith, R. Books are referenced by listing the authors last name first , the title of the book italics , the edition if other than first , the publisher followed by a colon , city and state if the city is small of publication, and the year of publication.
Other styles of referencing were used in the past and are currently used in other countries. References should be consecutively numbered, as encountered in the text x of the laboratory report. The reference number should either be superscripted or appear underlined in parentheses X following the phrase or idea that is. Failure to reference material obtained elsewhere constitutes plagiarism and isgrounds for immediate failure. Even if an idea from elsewhere is "put into your own words" rather than being directly copied or quoted, it must be ref- erenced.
Ebel, H. Schoenfeld, R. Kanare, H. Chapter 4 Literature Searching and the Inorganic Literature. We have included one question involving literature searching in each of the laboratory experiments in this text. In chem-. It lists and cross references the abstracts from all papers pub- lished in all major and most minor chemical journals.
The abstracts are placed into one of 80 sections within CA, depending on the subject matter contained in the referenced paper. The sections cover the following material:. The sections that are of the most direct interest to inorganic chemists are:. Articles of inorganic interest often appear in other sections, as well. The each weekly issue of abstracts are cross referenced in the index of CA by author, patent number, and subject keyword.
The weekly indexes are collected into six annual indexes, which cross reference the abstracts in var- ious ways:. Author Index. Lists all papers in alphabetical order according to the au- thor's name.
Chemical Substance Index. Lists all papers according to the proper name of all chemicals used in the paper. Formula Index. Lists all papers according to the formula of the chemical compounds used in the paper, in the following order: carbon first, hydrogen second, and then all other elements in alphabetical order. General Subject Index. Lists all papers according to subject keywords found in the paper.
Index of Ring Systems. Useful mainly for organic chemistry. Lists papers involving ring systems according to the type of ring system found. Patent Index. Lists all chemical patents in numerical order, as well as subsidiary patents. Every 5 years, a Collective Index is published in the past, it was every 10 years,and called a Decennial Index.
The 11th Collective Index is the current 3 one, with the 12th Collective Index now in press. These replace the Annual Indexes for the 5-year coverage period. Additionally, every 18 months, an Index Guide is published, listing all current keywords and chemical names used in the indexes. Searching a Topic in Chemical Abstracts There are several alternate schemes for searching a particular topic in Chemical Abstracts.
Two of the more direct methods are described next. Use of the Formula Index: Suppose, after doing Experiment 42, "Synthesis and Reactions of trans-Chlorocarbonylbis triphenylphosphine rhodium l ," you wished to see if the starting material, RhClH 2 0, had been used in the syn- theses of any other rhodium complexes. The easiest way to proceed would be to look up the formula in the Formula Index. The Formula Index lists formulas in the following order: carbon first, hydrogen next, and then all other elements.
Hydrates are listed under the parent compound formula. In this case, therefore, we would look under the heading CbRh. Generally, one begins a search in the most current volume of Chemical Ab- stracts, Volume as of this writing. Two references are listed under the sub-. The listing is shown in Figure 4.
These two references tell us to look up abstracts numbers , and , These abstracts are shown in Figure 4. In older volumes before , a different listing style was used. A typical abstract number for this period would be.
Cl 3 Rh Rhodium chloride RhCl 3 []. Chemical Substance Index trihydrate []. Chemical Abstracts formula index listing. Reprinted by penmission. A Literature Searching Van der Zeijden, Adolphus A.
Gerard; Nordemann, Richard A. Amsterdam, WV Amsterdam, Neth. Organometallics , 7 9 , Eng. The solid-state structure of I was detd. I two double consists of a Rh I center that has a square-planar coordination comprising the bonds of COD and a C atom and one N atoms of the monoanionic aryl ligand.
This process, which generates a highly unsatd. T-shaped 14 electron species, is accom- panied by the relief of steric repulsions within the complex. Structures of [ C 5 Me 5 RhCl] 2. Rauchfuss, Thomas B. Synthetic routes to tetrathiometalate complexes of rhodium, iridium, palladium, and platinum are described. Acetonitrile solns. COD PtCl 2 re- , , ,. The latter complexes reacted ,. The compd.
Figure 4. Chemical Abstracts abstracts listing. Reprinted by permission. In the collective volumes, the abstract number will appear as. Note that the compound we are searching for, RhCl 3 -3H 2 0, does not actually appear in abstract ,m Organometallics , 7, , although it does in abstract ,e Inorg. The reason. Any compound listed in the Registry Number listing in a paper will be cross-refer- enced in the annual and collective indexes of Chemical Abstracts.
This is a major advantage of the use of Chemical Abstracts the compound does not need — appear in the abstract to be cross-referenced. The abstracts provide a synopsis of the highlights of the papers, and one can then decide whether to look up the articles in the journals themselves. CA covers many minor journals, one frequently obtains listings in journals that are not available at a particular library. The Institute for Scientific Information also provides a document copy service.
The references found in the papers obtained in the search provide additional sources of information on the subject being searched. These references are not available in Chemical Abstracts, only in the paper itself. This is in contrast with the Citation Index see Section 4. Searching earlier volumes of Chemical Abstracts would provide additional papers detailing the use of RhCl 3 -3H 2 0. A Magnetic Susceptibility and 5. B Thermal Analysis , you wanted to see if it were possible to use thermogravimetric analysis to make magnetic sus- ceptibility measurements.
Since this is a question about general techniques rather than about a specific reaction or compound, the General Subject Index would be the logical place to start.
Consulting a recent General Subject Index, we could look up either "magnetic susceptibility" or "thermogravimetric analysis. A number of subheadings appear under the major heading "thermogravimetric analysis," one of which is " — use of in magnetic susceptibility detn.
This number tells you to look up abstract number , in volume of CA. Looking up these keywords in volumes show no additional ref- erences. One could carry the search as far back into the past as desired. Razo and R. Gomez, which appeared in in the Journal of Thermal Analysis, volume 34, pages The references cited within that paper would provide additional information about the given topic. The search may be conducted using various types of input, such as structures, molecular formula, CAS registry numbers provided in this text for all chemicals used , or keywords.
Advantages and Disadvantages of Chemical Abstracts: The Chemical Ab- stracts method of literature searching is the most common method for several reasons. Looking up a keyword or formula over a long stretch of time is very tedious. This is not a problem with or abstract, formulas, as the formula only need be listed in the Registry. Papers from all major and most minor journals are cross-referenced by use of authors, keywords, journal, location, and most im- portantly, by their references.
The SCI is now available on compact disc, which can be accessed using a personal computer. The printed SCI consists of three major parts:. Citation Index. Lists all papers as a function of the references they cite. Source Index. Lists all papers alphabetically, by the first author. Permuterm Subject Index. Lists all papers according to subject key- words. The computer version allows searches by the following criteria:. Cited Author.
The author of the reference cited by the article. The journal that the paper appeared in. Title Word. By subject keywords appearing in the title of the paper. The first step would be to enter the search using the subject keywords "thermal analysis" or "Rh III " in the latest issue of the Permuterm Subject Index. For the first 3 months of , there were 16 papers listed under the keyword "Rh III. The name would then be looked up in the Source Index, yielding the reference.
Electronic Materials 17 1 88 13R. The notation 13R indicates that the paper has 13 references. A code number for ordering the article would also appear after the 13R notation. This bibliographic information is followed by a list of the references cited by the paper, the first of which in this instance is. This indicates that the reference is by D. Barnum, and appeared in in. One would simply insert the CD into a disc reader, turn on the computer, and follow the menu to perform the search. In the previous example, using the word "Rh III ," the computer responds title.
These listings can be shown by title only, or the complete listing can be shown. More than one Title Word can be searched at a time, using logical commands such as "and" and "or.
In most cases, there is a well-known or not so well-known original paper on a given subject, which all subsequent papers are likely to cite. For example, if we were interested in the topic of "isomerism in transition metal complexes," the key papers were written by the chemist who pioneered this area, Alfred Werner. We would look up the name "Werner, A" in the Citation Index, and under his name would come a series of subheadings, each being a particular paper.
Under each subheading would appear a series of ref- erences to papers who listed Werner's paper as one of their references. In this way, we could quickly obtain a list of all papers on a particular subject area. The CD computer version is especially powerful.
Each listed paper also has a list of references and related papers. In the case of the paper by Poston and Reisman discussed previously, there are 13 references and 4 related records. The listing for the paper is shown in Figure 4. We can then list the 13 references found in this paper, shown in Figure 4. If desired, each of the referenced authors listed can then be searched to see if any paper abstracted in the given issue of the CD Citation Index cites any of their work.
We can also list the four related records, along with their references, an example of which is shown in Figure 4. A related record is a paper that has a reference in common with in this case the paper by Poston and Reisman.
In the case of the first related. The paper by Hassan et al. This would constitute a second-order search. Each of those 15 related records could then be searched in a third-order search, and so on. By using the references and related records, a huge bibliography of work on any particular subject can quickly and efficiently be built up. Typical Science Citation Index listing. Philadelphia, PA. Science Citation Index reference listing. Thus, once you have a key paper on a subject one all subsequent papers are likely to cite , searches can be accomplished without using keywords at all.
Older papers do, however, appear in the Citation Index. If the goal of the search is to obtain information on a given subject or chemical, CA will generally be easier to use. Since CA provides the abstract of the paper, the searcher can quickly determine if the paper obtained in the search actually is likely to contain the desired data. The two methods complement each other nicely, with CA generally being used for the initial search, and the SCI being used to obtain a broad coverage of the subject.
In addition to the journals, there are thousands of serial monographs and books published annually on the subject. Needless to say, it would be impossible to keep up with all of them! Selective literature searching solves part of the problem see Section 4. The most important information appears, however, in a relative handful of major journals and serial monographs, listed and briefly described below. Coverage has been restricted to major journals that provide at least abstracts in English.
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With over 45 experiments, Microscale Inorganic Chemistry incorporates the use of a broad sampling of elements and also covers such topics as laboratory safety, equipment, report writing, and literature searching.
New York N. APA: Szafran, Z. Microscale inorganic chemistry : a comprehensive laboratory experience. Set language NL EN.
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