Polarographic techniques - ACS Publications

which to manufacture school scientific apparatus. It is intended for manufacturers of apparatus and for workshops of vocational schools. The drawings ...
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JOURNAL OF CHEMICAL EDUCATION

THE CONSTRUCTION OF LABORATORY APPAWLTLIS FOR SCHOOLS

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H. Struers, Chemiske Lahoratorium, Copenhagen. United Nations Education, Scientific, and Cultural Organization, Paris, 1954. 76 plates. Many figs. Sizes vary. $8. for each Series.

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THIS bilineual .. Dublication (Endish .. and French). consists of a set of merbanirnl drawirrm thnt rnn hc wed i r the Murprint from which to mnnufacturr school scientific xpp:rnttus. It is inten~lrd for ~nanufncturrmof nppnmtus 2nd for worksltops of voc.!tiwd schools. The drawings of Series I are for general science apparatus. Series I1 contains directions for making 6 pieces of general apparatus, 25 items for mechanics, 7 for fluids, 6 for heat, 5 for light, 4 for sound, 17 for electricity and magnetism, 3 for chemistry, and 3 for biology. The chemical apparatus described includes a blowpipe, a pneumatic trough stand, and a water deionizinc column. ----~-The accompanying pamphlet describes the symbols used on the drawings, gives a list of the workshop equipment needed, and furnishes a list of the materials needed. ~

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ELBERT C. WEAVER

P m r ~ r Ac*owr ~s A ~ o o v ~M n ,* a s * c ~ n s s r ~ I

METHODS OF QUANTITATIVE MICRO-ANALYSIS

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Edited by R. F. Milton and W. A. Woters. St. Martin's Press, 742 pp. Figs. and tables. 16 X 23.5 New York, 1955. xi cm. $15.

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r~~~~~~~~ OF Q~~~~~~~~~~~ ~ - ~ - - -M - - - - -~ is the result ~ of an ambitious and laudable attemptto present, in one vol&ne, much of the pertinent information concerning a variety of specialized micro techniques. The volume is composed of seven parts. Each pmt has been contributed by one or more specialists and containins a brief discussion of theoretical principles, description of apparatus, and details of manipulative technique. In many instances, examples of the application of the technique to the analvsis of soecific materials are described. A table summarieinn the metiods of anslvsis and contilinine literature ~-~~ references concludes each part. Part I, on gravimetric techniques was contributed by R. F. Milton, W. A. Waters, and G. Ingram (pp. 11-55). Use of the micro balance, drying of samples, filtration methods, use of the centrifuge, and separation by dialysis are discussed. Notes on the use of organic reagents for the gravimetric determination of metal8 are also included. The treatment of weighing, as illustrated by the given example, is judged as inadequate. Part 11, "Micro-analysis of organic compounds," by W. A. Waters and G. Ingram (pp. 57-133) discusses the quantitative elementary analysis of organic compounds, the determination of functional groups, and molecular weight. For the determination of carbon and hydrogen, combustion tubes packed with Ingram's boat filling are apparently refo or red to tubes ~ a c k e dwith Precl's ~

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era1 miucioles. de$'ohotion of &maratus. and exoerimentd tech, niques. A wide vnrit.1). of evrrllent rxnmplcs of the hpl,lir%ricn of the micro-~olumrtriepro,:edltrcs are d*.scr~IwI. i~" F.I rhlilton(l,p220-12ll), ~ Part IV, ' C ( o l o ~ i m ~ 1 T i r ~ n n I y ~It. is devoted t o a discussion of general principles and the apparatus used for colorimetry, nephelometry, and fluorimetry. A considerable number of examples of colorimetric analysis are cited. The description of their application to the analysis of biological materials, water, gases, organic compounds, trace quantities of metals, etc., is brief and adequate for measurement with visual apparatus. The value of both this part and Part I11 would be enhanced had the author included a discussion of the importance of conducting blank determinations along with the sample analysis, especially when appreciable quantities of reagents are used,

as in wet ashing procedures. Some information about the selection of stable standard substances and the necessity of assaying stock solutions made of substances which are subject to chsnae d u r i u PIOrnge ~ should ~ H V Iwen Q uoted. l'nrt V, 't.lectr~cl~emieul methods of mirn+mlyris," by J. 'T. Stock (rw. , 421-XUI. ewers the theon' and aunlimtion of rmrntiomctry, polnrugmphy, elertrodrpo+ion, coulornctry, conducri~netricnnalvsis, :lid elertrol,horr4~. Sunmuus tables, graphs, 2nd illusrrntions of vnrioua l,i+cn of nppnrntus accompany lhr text. Part VI, "Gasometric methods of micro-analysis," by K.M. Wilson (pp. 521-605), describes the novel and clever techniques of Blacet and Leighton, T. C. Sutton, and R. Spence for the analysis of common mixtures of gases. The glycerineentrained bubble method as applied to the analysis of gas bubbles occurring in glass is also described. Application of the Van Slyke apparatus the Warburg apparatus, and the Barcraft differential resperometer is explained and typical examples of analysis are cited. Various tables and charts for use with the Van Slyke apparatus are included. Part VII, "Chromatographic analysis," by S. M. Partridge and T. Strain (m. 608-30). is a condensed discourse on chromatagraphic techniques and their applioation to various types of analy~is. Various techniques, theoretical principles, and apparatus are briefly treated. Good examples of the ~pplicationof ionexchange methods, paper chromatography, partition chromatography, and adsorption chromatography are given. This section is a good introduction to the field of chromatographic analysis. Part VIII, "Biological methods of micro-anelysis," by A. J. Amos (pp. 68%91), is concerned mainly with the determination of various vitamins and amino acids. Apparatus, procedure reauirements. and severalexam~lesof analvses are brieflvdescribed. Basic training this branch ~ in brtoteriology ~ is a prer&isitefor A ~ of analytical work. This volume serves the editors'purpose wellby making accessible t o the average laboratory worker information about techniques whioh previously have not been readily available. Both the editors and the contributors are to be congratulated for their effort in accomplishing such an arduous and difficult task. The book should prove a vduable acquisition of most analytical laboratories, especially those whose function is to perform a diversity Of ILnalyses. HARRY T. JOHNSTON P. S A D T L61~ SON.INC. SAMUEL

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P m ~ r o e ~ ~ wP r *s a , ~amv~m*

POLAROGFSPHIC TECHNIQUES Louis Meites, Assistant Professor of Chemistry, Yale University. 317 pp. Interscience Publishers, Inc., New York, 1955. xiii 33 figs. Tables. 15.5 X 23.5 cm. $6.

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THISis an exr~.llmtbook for those vhu wnnt tu ltuw n short 2nd dear introrlurrion to tllrorericnl 2nd prrrtirol pol-irography. \Vrittcn primarily :m a wxtbook, i t fill* n w r y rml nerd in the polarographic literature.

inclided, bne on trouble shooting in polarographic' circuits and the other a tabular oompilation of half wave potentials and d f i sion current constants of inorganic substances. References t o the original literature are provided. Theoretical principles are covered in four chapters. The topics considered are the residual, migrat.ion, and diffusion currents, kinotio and catalytic currents, adsorption waves, theory of the current-voltage curve, criteria. of reversibility, interpretation of half wave potentials and maxima. A knowledge of the fundamental theory common to polltrography and all other electrical methods of analysis is assumed. Four chapters me devoted t o more practical considerations. These are instrumentation, techniques of quantitative polarographio analysis, amperometric titrations, and special techniques. The last of these discusses

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VOLUME 33. NO. 4. APRIL, 1956

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controlled potential electrolysis, coulometry a t controlled potential, microcoulometry, and derivative polarography. The brief discussions of kinetic and catalytic currents, adsorp tion waves and interpretation of m a x i m are in keeping with the introductory nature of the book. In this respect the author has done an excellent job of keeping the discussions concise while adequately covering the more important theoretical foundations of polarography. The experiments found a t the end of the chapters are well chosen to illustrate the principles considered in the text. The chapters dealing primarily with techniques offer many valuable suggestions to those having little or no experimental experience in polarographic techniques. In addition to the inclusion of classical amperometrio titretions, a discussion of the techniques and interpretation of amperometric titrations with two identical indicator electrodes and potentiometric titrations at constant current with one or two indicator electrodes might have been given, since the interprets, t,ion of these titrations is based on current-voltage curves of the substances involved. This book will be welcomed by students, teachers, and research workers alike as an excellent textbook in polarography and as a valuable guide for experimental work. RICHARD C. BOWERS

topics clearly presented. Tables of solubilities, atomic weights, and the periodic table are given inside the back and front covers, making them easily available to the student. In addition, eettine two books for less than the usual mice of one would be a welcome change for most students. The system of analysis follows the traditional hydrogen sulfide method. The Bronsted theory of acids and bases is followed and is presented in a separate section in the chapter dealing with ionization. Its applications to hydrolysis, amphaterism, snd complex ions are treated in separate sections in the chapters dealing with these topics. Certain other topics are also treated in this way, making it possible to omit them without destroying the continuity of the bulk of the material. This makes it possible to use the text not only in a. separate course in qualitative analysis hut also as part of the first-year general chemistry which includes qualitative analysis, but in which there may not be time to deal wit,h all of t h r v topics. n a t h r r iuch scction contins qr&l proredures for fcrro- and hioh-nluminum slloys. Tllir is imiqtw katurc of rhc text wl.irll orovidcs rhr inrtructor with 9 mmnc c,f modiirine. the general of the laboratory or providing dditibnai material far special groups such rts the more advanced, rapid, or sifted fit,ndent,s.

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Non~~wesU r ~~nr ~~ ~ ~ s r r r EVANBTON. ILLINOIB

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QUANTITATIVE ANALYSIS: METHODS OF SEPARATION AND MEASUREMENT

M. G. Mellon, Professor of Analytibal Chemistry, Purdue Uni694 pp. versity. Thomas Y. Crawell Co., New York, 1955. x Figs. and tables. 16 X 24 cm. $6.50.

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T ~ r book s is divided into three main sections: I. General Prinoiples, 11.Laboratory Exercises, 111. Problems. In the first section, sampling and separation processes are discussed a t length with individual chapters on separation by volatilization, precipitation, electrochemical, and partition processes. The second part of the section deals with the problem of measurement withespecial emphasis on titrimetry and chapters on colorimetry and electrometry. In the laboratory section, a library problem is found in addition to a. considerable number of laboratory determinations. The discussion of the treatment of experimental data includes an introduction to confidence limits and control chartt. The book oovers a rather wide range, from elementary points of technique to a good treatment of photometric analysis. I n this broad coverage, some detail is necessarily sacrificed and the author has chosen to minimize the theoretical discussion and calculations of ionic equilibria on the basis that these are mastered in qualitative analysis. This assumption might be questioned in view of the diminishing role which qualitative analysis plays in some onrriculs. The organization of the book is such that in the laboratory exercises as well ss in the theory somewhat advawed subjects precede more elementaly ones. This may create problemsfor the tertcher of less mature students.

more problems on his own. This reviewer believes that answers to odd problems are sufficient, giving the instructor more flexibility in their use, and preventing the student's working "toward answers." A. A. MEYER

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NEW METHODS IN ANALYTICAL CHEMISTRY

Ronald Belcher, Reader in Analytical Chemistry, University of Birmingham, and Cecil L. Wilson, Reader in Analytical Chemiskv. The Oueen's Universitv of Belfast. Reinhold Publishino CO&., ~ e w -Yark, 1955. 2 287 pp. 1 fig. 10 tables. 14.5 X 22 cm. $5.50.

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W ~ n 81 r new gravimetric and volumetric analyses based upon 385 research articles published chiefly during the last 20 years, this book will be a valuable source of information to any chemist with analytical problems. New advances in the classical analytical methoda tend to be overshadowed by the present trend toward instrumentation, hut these advances are being made and this book mtlv , describes them. New gravimetric and titrimetrie methoda are given for the elements Al, Sb, As, Ba, Be, Bi, Br, Cd, Crt, CI, Co, Cu, F, Ge, I, Fe, Pb, Li, Mg, Mn, Hg, Mo, Ni, Pd, P, K, Rb, Se, Si, Ag, Ns,S, Te, TI, Th, Ti, W, V, Zn, and Zr, and for the ions of ammonium, hromate, bromide, chlorste, chloride, cyanide, dichromate, ferrieymide, fluoride, iodate, nitrate, permanganate, LUCY W. PICKETT persulfate, sulfate, sulfide, sulfite, thiocyanate, thiosnlfate, and M o o m H o ~ r o COLGEOE x~ vanadate. New methods are also eiven for the determination of , ~sa~c~nam~Ta S o m n H m ~ r ; uM hydraaine, hydrogen peroxide, p&nylhydr&zine, and sulfurous acid and for the calcium hardness of natural water. Other sections are included on indicators, extractions, and multipurpose 0 SEMIMICRO QUALITATIVE ANALYSIS and other reagents. The list of new organic reagents ia imposing. Edwin 0.Flagg, University of Rochester, Willard R. Line, No claim is made by the authors that the book covers the field University of Rochester, and John F. Flagg, Knolls Atomic Power completely to date, nor have they personally checked all of the Laboratory, General Electric Company. D. Van Nostrand Co., methods described, but they have done so with a reasonable New York, 1954. viii 238 pp. 15.5 X 23.5 cm. 53.25. number of them while others have been included which were recommended to them by investigators repute. THIScombination text and laboratory manual is a revision of looking far of recent research in gravi~l~~~ and ~i~~ u ~ ~~ ~~ i ~~ ~ l ~ i li ~ ~FOT. ~i ~those ~ ~. w ~~ i an~evaluation ~ the metric and volumetric analysis, this book should prove most while the book has been completely rewritten with a ably expended theoretical section, it retains the experimental helpfu1. procedures and much of the form of the earlier one. V. R. DAMERELL This book seems to be written with the student in mind. The WE,,.,, R E ~ E ~ VUEN I V E R B I T ~ CLEYELAAD, OHIO large type is easily read, the illustrations quite lucid, and the

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