A manual for the organic chemistry laboratory - ACS Publications

two dimensional chromatograms or ... this challenge, the authors submit two new schemes for qualitative analysis based solely upon paper chromatograph...
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JUNE. 1954 of inorganic analy~isby means of filter paper and cellulose powder chromatography. The ten chapters of this monograph have heen written from a practical point of view. The various procedures and apparatus used are nresented in sufficient detail to enable the worker to cnrn nut qualitative and quantitstivr snnlyrrr. Only a brief, nonmnthrmnricnl account of the furtdnrnrntnl ilwuriw, prinviplw, and f:w~,rr.~9tlwy arc xpplirnhle to inorganic chronum,yrn~,hy is given. A complaint of the uninitiated is that not enough information appears in publications to enable them to duplicate the experiments. The sllthon rectify this in three clearly written chapters, Techniques for Preparing Chromatograms, Location and Identifieetion of Zones, and Choice of Solvent and Separation of Cations. The four decisions that confront the worker before starting his chromatogram are fully discussed. These are: (1) the type of paper or cellulose powder to be used, (2) the kind of a p pssatus to be employed, (3) whether one or two dimensional chromatograms or a cellulose column is to he used, (4) the solvent mixture to he used as the mobile phase. The authors have also succeeded in relieving one of the biggest headaches in chromatography, namely, the location and the identilication of aones of the separated ions. They have presented in a lucid and concise manner many inorganio and organic reagents which can be used as distinguishing tests of varying sensitivity for the majority of the cations. These chromogenic reagents are classified as (1) general reagents for the location of many cations, and (2) special reagents which may be specific for one cation, or poseihly a small group. In addition to the chapter on solvents, extensive tables are compiled in an appendix, listing some 110 solvent mixtures, the ions separated, Rf values, comments, and references. I t has been stated that "in spite of extensive investigations, chromatography has not provided a systematic anslytical procedure for mixtures of many different inorganic substances. Multieomponent mixtures are commonly resolved into groups by conventional chemical methods, and these groups are then resolved by chromatography based upon adsorption, partition, or ion exchange." To answer this challenge, the authors submit two new schemes for qualitative analysis based solely upon paper ehrometography without any previous separation by ordinary chemical methods. Detailed procedures for the separation and id~ntificstionof 30 cations by these schemes are given. An appendix at the end of this chapter gives a list of analytioal reagmts used. The principles for the resolution and the identification of anions are not as rlearlv h o w n as those for the oations. A systematic scheme of analysis for anions is needed to complete the plcture of inorganic chromatogmphy. A limited scheme of analysis for about 28 anions devised along the lines suggested by M. Lederer is presented. Also extensive details are given for the quantitative investigation of condensed phosphates according to the researches of Dr. A. E. R. Westman. Typical examples are given to illustrate how chromatography, in conjunction with colorimetry, polarography, or mierotitration, can he used for the quantitative estimation of microgram amounts of cations separated from inorganic mixtures. Some of these methods are now standard operational &assayprocedures. The authors state, and prove their contention by giving examples and references, "that sometimes it is advantageous to combine the use of cellulose with that of other supports." This is the resson for their chapter on Chromatography Using Other Media Than Cellulose. The book closes with a. chapter on the current research favorite, electrochromatogrephy, especially as a. means for the continuous separation of materials and as an analytioal tool. Techniques, typical apparatus, etc., are given in detail. The material in "Chromatographic Methods of Inorganic Andy&" is well organized, clearly written, and replete with many illustrative exmnples. The printing, paper, binding, and typogranhv are excellent. (A minor error resultine from a trans-

333 piece.) The format is such that the reader can, without any difficulty, look up any particular point with which he may be eancerned at the time. The inclusion of an appendix at the end of the chapters on the Choice of Solvent and Separation of Cations and the Analysis of Unknown Mixtures of Cations keeps the main presentation nnenoumhered and at the same time makes available to the reader additional information pertinent to these phases. This hook is recommended by the reviewer not only to the beginner but a180 to the industrial chemist and the researcher who may be interested in using this important research and analytical tool. JOHN G . SURAK

A MANUAL FOR LABORATORY

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THE ORGANIC CHEMISTRY

Leigh C. Anderson and the late Werner E. Bochmann, Pr* fessors of Chemistry, University of Michigan. John Wiley B Sons, Inc., New York, 1953. mi +'I64 pp. 22 X 27.5 om. $2.75. FIRST,it is this reviewer's rare privilege to testify the worth of this book from his experience as a student who used it in his first course in organio chemistry. Then, in 1940, it was s n earlier edition published by Edwards Brothers, Ann Arbor, Michigan. This reviewer remembers it as a very satisfactory lab manual; indeed, it was one of the faxtors which shaped his interest in a career in organic chemistry. In his present capacity as a teacher, he still feels it is a good e manual., almost entirelv hook. It is a traditional t .v ~ of , conw r r d witl, pn.par.ttwr r~pcrinlmt.;and dmling with aliplmtir elwmi,try at Ihg111 lwiore any :tnm,& rornpounds an. prcptrrd. , 1 1 1 ~ 1instead 01 lh