摘要:

January, 19661 SHORT PAPERS 55 SHORT PAPERS Detection and Estimation of Ethylene Glycol in Propylene Glycol by Thin-layer Chromatography BY H. B. S. CONACHER* AND D. I. KEES (The Lyons Laboratovies, Haminersmith Road, London, 14’. 14) PROPYLENE glycol is used widely as a solvent for pharmaceutical purposes and flavour forniula- tions. The limitations in the number of published specifications and their deficiencies in testing for impurities of a glycol character have already been revicwed.l A tcst bascd on the determination of the critical-solution temperature of propylene glycol and ether, that detects 0.1 per cent. of ethylene glycol or similar amounts of water in propylene glycol has been described.1 However, as ultra-dry ether must be used, the test is not appropriate as a routine method for detecting trace amounts of ethylene glycol in propylene glycol.Thin-layer chromatography was considered to be the most suitable technique, but the various systems described in the literature that claimed to separate the two glycols proved to be un- suitable. This was due either to streaking of the spots2 or to the too low R, values obtained that resulted in littlc or no ~eparation.~ A clear separation was finally obtained by modifying Knappe’s solvent,3 by using acetic acid in place of formic acid and increasing the acid content from 3 to 6 per cent. Of the various reagents recommended for detecting glycols,2 none proved to be as sensitive as a modification of the periodate - rosaniline hydrochloride r ~ a g e n t , ~ that could detect 0-5 pg of ethylene glycol.The method described can detect 0.1 per cent. of ethylene glycol in propylene glycol; the same levels of glyccrol can also be detected. Visual comparison of spots affords an estimation of the ethylene glycol content to the nearest 0.1 per cent. (see Fig. 1). METHOD REAGENTS- Rosaniline hydrochloride solution-Dissolve 1 g of rosanilinc hydrochloride in water, and make the solution up to 100 nil. Bubble sulphur dioxide through it for 5 minutes, and allow the solution to stand for 30 minutes. Add some active carbon, then shake and filter the mixture. A pale straw-coloured filtrate is collected. Periodate solution-Dissolve 2 g of sodium metaperiodate in 100 ml of water. PREPARATION OF PLATES- Shake 70 g of aluminium oxide G (E. Merck, obtainable from Andcrman & Co.Ltd., London) with 100 ml of water for about 3 minutes, and apply the resulting slurry to glass plates (SO cni x 20 cm) a t an applicator sctting of 500 p. Allow the plates to dry in air overnight, and use directly. PROCEDURE- Prepare standard 10 per cent. w/v ethanolic solutions of propylene glycol containing 0 to 1 per cent. w/w ethylene glycol with respect to propylene glycol, and also a 10 per cent. w/v ethanolic solution of the propylene glycol sample whose ethylene glycol content is to be deterniined. Spot 5-pl aliquots of these solutions 1.5 cm from one edge of thc plate, and develop with a mixture of chloroform, toluene and acetic acid (77 to 17 to 6) for 14 hours in a tank lined with filter-paper soaked with the solvent mixture.Allow the plate to dry for a few seconds, spray it lightly with the periodate reagent and after allowing the plate to stand for about 1 minute, spray it with the rosaniline hydrochloride reagent. Propylene glycol, ethylene glycol and glycerol appear as dark purple spots about 50 mm, 27 mm and 5 mm from the origin, respectively, on a pink background that slowly darkens on standing. Examine the plate for the presence or absence of a purple spot from the sample slightly below the large purple spot due to propylene glycol. If a purple spot is visible, compare it visually with the ethylene glycol spots from the standard and estimate the amount present in the former. If a spot is also observed near thc origin, this is an indication that glycerol is present. * Present address : Department of Chemistry, St. Salvator’s College, St. Andrew, Scotland.Fig. 1. Chromatogram of propylene glycol containing 0 to 1 per cent. of ethylene glycol on alumina, after 18 hours’ development. [ t o face page 5556 SHORT P4PERS iAnaZyst, Yol. 91 I~EFERENCES 1. 2. 3. 4. ?Iliddleton, G., and Stuckey, I<. E., Awdyst, 1950, 75, 406. Wright, J., Cheun. & Ind., 1963, 1125. Iinappe, E., Peteri, D., and Iiohdewald, I., 2. aizal. Ckern., 1963, 199, (4), 270. Baddiley, J., Buchanan, J. G., Handschumachcr, I<. E., and Prescott, J. F., J . Chein. Soc., 1956, Received JrtZy 16th, 1965 2820.

ISSN:0003-2654    

DOI:10.1039/AN9669100055

出版商:RSC    

年代:1966

数据来源: RSC

摘要:

56 SHORT P4PERS iAnaZyst, Vol. 91 Apparatus for the Equal Distribution of Colour Reagent on Chromatograms Used for Quantitative Work BY IV. LOUWERSE (Institute fov Biological and Chemacal Research o n Field Crops and Herbage, IVagenzirgeiz, The Nethedaizds) Ir; order to develop a colour on paper chromatograms the paper is usually sprayed with the reagent. This method is not very useful in quantitative work, as it is djfficult to distribute the substance uniformly. I n quantitative work on amino-acid chromatograms this method gave irregular results. To overcome the difficulty Tocnnies and Kolbl pulled the amino-acid chromato- gram through a solution of ninhydrin in acetone. As amino-acids are insoluble in acetone, running is prevented. In testing this method it appeared that the colouring o f the amino-acids was irregular and some amino-acids such as y-amino-n-butyric acid gave no colour a t all.A better reagent is a 0.5 per cent. solution of ninhydrin in a water-saturated mixture of butanol - acetic acid, 93 to 7, as used by Linskens,2 but this has the disadvantage that the amino-acicls are slightly soluble in it and start to run when the paper is too wet. This is common with the so-called “dipping” technique, in which the paper is pulled quickly through the solution. A method for using this reagent was developed in which a uniform distribution of the reagent is achieved without running of the amino-acids. As the technique proved to be successful a brief description is given. METHOD The chromatogram is pulled between two glass rollers, about 7 0 cni long and 2 cm in diameter.The lower one, C, dips in a trough, -4, filled Both rollers are covered with “tubegauz” bandage.* 5 670 A = Glass trough B = Bearing for roller C C = Roller with bandage D = Bearing for roller E E = Roller with bandage F = Wooden frame Fig. 1. Diagram of the apparatus. All dimensions are given in millimetres * The Scholl Mfg. Co. Ltd., London, E.C.1.LOTH“ ’ a: ’ W” 0 Fig. 1. continued. I I I CHX3-CI, Br 40 P HC-OCH,, H C - N(CH3)Z CH CQ0 ‘H 40 0 p CH3CHzC,H + CH30CzH -CH,CH=CH-C. ‘+I ,O ‘H PhC ’ X-PhCQ0 CI, CH,O, N(CH,), ‘H - 40 /p RC-OH+ PhC-OH RS03H, -,- PhS0,H I D I I m(CH3)4Si * C H3(CHz),C H3, (C Hz.),CHz,(CH3)3CH,(C H3)4C H3(CHz)zOR, (C H,),C(OR),, CH,C(OR), R E . CH,SH, (CH3)zCHSH Ca(CH,), n = 2, 3,4, 5, 6 , - >N, NOR, COOR, NR, - COCI, c=c, Ph, OR I (CH313C H C H ,-C-X (CH,),CH-X - CI, Br, I CH,CN __ RNH,, R,NH H,C-----CH, e-r), H ~ c ~ H , .6 1 CH, =C(C H3)Z - CHO, COR," COZR, OCOR (CH,CO),O - _ _ _ ~ o=c (CH,),N-X CHzPh, CHZOH, CHOP Ph (CH,),O, (CH,),N, (CH,)zS H-Q-H, H ~ H , H ~ H - - - CH,-X - )N (acyclic), )N (cyclic sec.) -CH,-X ->N (cyclic t e r t . ) , NHCOCH,, )CH-X 1- NHSO,Ph, Quart. salts -CH,NH,, )CHNH, C H ,Ph CH,CH,Ph, PhCH, CH,Ph, (CH,),CHPh Fig. 1 I L E l I rn I I I - I rn I I m I I i I r O'I G H , ,,C:H, , b c H z =C-CH2-X- C=C, -C<' Br, OH H ' 0 CH3CCHz-X - COOCH,, COCH, PhNHz >CH-X I I I IJanuary, 19661 BOOK REVIEWS 57 with the reagent (see Fig. 1) ; the upper roller, E, is filled with water, to make it heavier and so press more tightly against the other.Both rollers are suspended on horse-shoe shaped glass bearings, B and D, so that they are free to move in a vertical direction. When the bearings and the rollers are placed in a wooden frame, F, the two rollers, covered with the bandage, just touch each other, while each rests in its own bearings. Further details and the exact dimensions (in mm) are given in Fig. 1. The bandages around the two rollers are evenly wetted with the reagent by a few turns and the chromatogram is pulled through. The chromatogram becomes uniformly wetted, but the amount of reagent in the paper is so small that no running occurs and the spots can be located exactly. If the upper roller, E, is not filled with water its weight (150 g) is insufficient to ensure uniform wetting of the paper. When filled with water it weighs 250 g and gives good results. Papers other than Whatman No. 1 have not been exanlined for colouring and wet strcngth. The amount of reagent dispensed may depend on the roller weight, but is not critical as long as the paper becomes uniformly wetted. An extra loading up to 450 g does not affect the results. REFERENCES 1 . 2. Toennies, G., and Kolb, J . J . , Analyt. Chem., 1951, 23, 823. Linskens, H. F., " Papierchromatographie in der Botanik," Springer-Verlag, Berlin, 1955. Received April 27th, 1965 Characteristic Nuclear Magnetic Resonance Spectral Positions for Hydrogen in Organic Structures BY E. MOHACSI (Department of Chemistry, Harvard UniversitJV, Cambridge 38, Massachztsetts, U.S.A .) THE table reproduced as Fig. 1 is proposed for quick qualitative interpretations of chemical shifts ( 7 ) relative to tetramethylsilane ( 0 = 10 - 7 ) . Received March 17th. 1965

ISSN:0003-2654    

DOI:10.1039/AN9669100056

出版商:RSC    

年代:1966

数据来源: RSC

摘要:

January, 19661 BOOK REVIEWS 57 Book Reviews ORGANIC COMPLEXING REAGENTS : STRUCTURE, BEHAVIOUR, AND APPLICATIOK TO INORGANIC ANALYSIS. By D. D. PERRIN. Pp. xii + 365. Kew York, London and Sydney: Interscience Publishers, a division of John \%ley & Sons Inc. Few books have provided a greater stiniulus to research in the field of organic analytical reagents than Feigl’s “Chemistry of Specific, Selective and Sensitive Reactions.” Published in 1949, this hook retains a considerable value to the research worker, but is becoming unavoidably dated, and all the subsequent, extremely interesting developments in this subjcct remain scattered throughout the literature. In commissioning Dr. Perrin to write a volume on organic coinplexing reagents, the editors o f the Interscience “Chemical Analysis” series have recognised this great deficiency in the literature of analytical chemistry.The result is a well integrated text describing the structure, behaviour and application to inorganic analysis of most of the significant reagents developed over the past 15 to 20 years. In presenting the basic principles on which the application of organic analytical reagents depends, the author has drawn freely on his knowledge of modern theoretical inorganic chemistry and has successfully indicated how reasoned empiricism can lead to the development of analytically useful reagents. As with Feigl’s classic text, the present book makes no attempt to provide practical details, but rather indicates the nature and types of reagents available for particular purposes. To some this may prove a disappointment, but the value of the book to the analytical chemist lies much more in its presentation of the philosophy underlying the development and application of organic reagents, than in any provision of procedural details of actual methods.All too often, the analyst makes use of organic reagents without fully appreciating the reactions involved, and this book does much to eliminate this empirical approach to reagent chemistry. 1964. Price 90s.58 BOOK REVIEWS ;Analyst, Vol. 91 This interesting and stimulating book must prove indispensable not only to the seekers of new and move usefuE reagents, but also to the users of these reagents who so often are bewildered and confused by the immense variety of apparently complex organic compounds now a t their disposal.The recent literature has been thoroughly covered to make this a very comprehensive text worthy of the most careful attention. Although one cannot imagine it supplanting Feigl’s book-with its intense projection of the author’s experience and personal philosophy-never- theless, the present book goes a very long way towards providing a thoughtful and up-to-date account of the subject. I n warmly commending this book to all analytical chemists, the reviewer syiiipathises with Dr. Perrin in the concluding paragraph of his text, and offers a further quotation to stimulate the researchers: “There is something in this more than natural, if philosophy could find it out.” The perfect reagent, perhaps ? ~TILLIAM I. STEPHEN COULOMETRIC ANALYSIS.By Dr.phi1. KARL AUIZESCH and 1)ipl.-Chem. IKGEBOKG CLAASEN. Translated by L. L. LEVESON. Pp. xii + 275. London: Chapman & Hall Ltd. 1966. Price 36s. This is a translation of the German text of 1961 (Nonogrnplrzen zu “ilngewanllte Chemie” uizd “Cliemie- Tngenieuv-Technik” No. 7 1 , Verlag Cheniie). there is no significant alteration, there is little to add to the review of the original edition ( J . Roy. Inst. Clieuz., 1961, 85, 365). KO more than a dozen of the five hundred odd references are of 1959 vintage, so that the prolific literature of the past seven years escapes attention. One additional reference (from 1959, without a title) has been included, although this is in the form of a correction which is already covered in the citations.One citation from a book has bccn replaced by the new edition, but otherwise the bibliography is untouched, having the same abbreviations, capitalisation and non-standard journal titles, The appendix on historical development has been transferred to the beginning and incorporated in the introduction. A circuit diagram of the, now classical, Boonian potentiostat-integrator has been inserted, without any textual explanation, and acknowledged to Verlag Chemie, although i t is reprinted from a U.S.A.E.C. report. Many of the diagrams have been reduced in size, and some turned sideways, because of the smaller page size, and German annotations have been translated, although symbols remain unaltered. The reproduction has thickened the lines of the drawings, but is good.The tabulation of the symbols used in the text has been removed without disadvantage, and some symbols have been replaced by more familiar ones. Sonic explanation of the I.U.P.A.C. sign convention and of formal potentials (which arc not further pursued) has been inserted, and there are a few minor insertions and omissions, as on p. 173 where a useful, if obvious, corollary is omitted, and some changes, as on p. 11 where “polarisable” has become “polarised. ” This book, therefore, gives a reasonable account of the state of the art in early 1959, when generation and titration efficiencies were beginning to be sorted out, background currents were beginning to be understood, and operational amplifiers were beginning to emerge from analogue computers into wider fields of application.Much of it is still relevant and accurate, but much, particularly on the instrumentation side, is obsolete. .As a guide to the earlier literature and to the simpler methodology i t still has undoubted value, and will be welcomed as such, but the severe limitation of its coverage is a defect that could be overcome only by complete rewriting and a great expansion in size. AAs i t is, i t offers a careful and successful translation of a useful short introductory monograph on an important subject. The book is produced by photo-litho from a Vari-type manuscript, which no doubt accounts for its very reasonable price. Many English papers retain German titles, and some errors have crept in. E. BISHOP IXTERPRETATION OF NMR SPECTRA: 1 1 ~ EhlPIKICAL APPROACH.By ROY H. BIBLE, JuN., Ph.D. The advent of high-resolution nuclear magnetic resonance spectroscopy in the last 10 years as an invaluable spectroscopic technique for chemists has brought with it a steadily growing library of text-books on the subject. This latest book is different in many ways from similar books. As its title implies, it deals with the interpretation of high-resolution nuclear magnetic Pp. x + 150 + folder. New York: Pleiiuni Press. 1965. Price $12.50.January, 19661 BOOK REVIEWS 59 resonance spectra from a completely empirical standpoint with scarcely a mention of the theory of the nuclear magnetic resonance phenomenon. The preface to the book states that its two main objectives are to guide organic chemists in the interpretation of proton magnetic resonance spectra and to provide reference data to aid such a task.N7ithin these rather limited terms of reference the book fulfils a most useful purpose. The book commences with a very brief discussion of the scope, limitations and applications of nuclear magnetic resonance and then goes on to consider in more detail the various fundamental features of proton resonance spectra. The relationship of chemical-shift values of absorption lines to electronic screening effects is dealt with, and a chart correlating characteristic chemical-shift values with nuclear environments is discussed. A useful feature of the book is that a larger version of this correlation chart is housed in a pocket on the inside back cover, thus enabling the chart to be put to everyday use.The spin-spin interaction phenomenon is discussed in very simple terms, together with tables showing characteristic spin-coupling constant values for protons on saturated systems, multiple bonds and aromatic systems as well as some examples of long-range spin-spin interactions. The relationship of the coupling constant of protons on adjacent carbon atoms to the dihedral angle is also mentioned. The author then goes on to discuss the origin of first-order spin patterns and warns against confusing bands split by spin-spin interaction with those split by an internal chemical shift due to non-equivalence of the protons in question. The interpretation of some higher-ordcr spin systems (e.g., AB and ABX types) is then dealt with. The treatment here is fairly detailed, but again quite empirical, with no mention whatsoever of the quantum-mechanical origins of the observed spectral patterns of such systems. The treatment is thus necessarily superficial, but consistent with the aim of the book.It is a pity, however, that space was not found for dealing with two other commonly occurring higher-order systems, namely the AB, and ALX; types. The book does include a brief mention of techniques useful in simplifying spectra, such as multiple resonance methods, and ends by suggesting a systematic approach to the interpretation of all types of nuclear magnetic resonance spectra. The book is written in a clear and lucid style and there are numerous summaries in each chapter of the essential points in the text. This will be particularly suitable for the preparative chemist who is concerned with the essential facts of spectral analysis rather than their theoretical origin.Unfortunately, however, the high pricc of such a small book will strongly deter the organic chemist with only a slight interest in nuclear magnetic resonance froni purchasing it. As the book is specifically aimed a t such people, this rather defeats its object. The book also contains an appendix giving a suggested operating procedure for the Varian A-60 spectrometer, which is rather out of place in a general text-book. K. G. ORRELL HIGH-TEMPERATURE COMPOUKDS OF RARE EARTH METALS WITH NONMETALS. By GRIGORII VALENTINOVICH SAMSOSOV. Pp. xiv + 280. New York: Consultants Bureau. 1965. Price $17.50. In this book the author discusses the data that have been assembled on thc properties and potential fields of application of these compounds which so far have received limited attention. Investigations of the solid-state reactions leading to methods of preparation are extensively covered.It is useful to find a monograph whcre physical properties, chemical properties and elcctronic and crystal structures are featured together. The delay involved in translating the work from the Russian (and presumably for the liussian author’s translation of \Vextern papers) has made one or two sections out of datc-particularly that on the carbides. The author docs not mention certain papers published in the period from 1961 to 1964-including those conflicting with his own work. In view of the difficulties in obtaining pure compounds of these types, a more critical approach to the early work would have been desirable.Frequent spelling mistakes and omissions (both in the text and the references) indicate inadequate editing of the translation, whose often stilted style could have been improved simply by re-phrasing the English. The abundant data on physical properties make this work of particular interest to the technologist-reports in unIamiliar Soviet journals are well represented. Spedding and Daane’s “The Rare Earths,” 1961, and Orchneidnev’s “Rare Earth Alloys,” 1961, cover some of this field, but do not attempt to be so comprehensive. This book can therefore be recommended, mainly because there is no adequate counterpart in the Western literature. G. NICKLESS60 BOOK REVIEWS [Analyst, VOl.91 FORMULA INDEX TO NMR LITERATURE DATA. Volume 1: REFERENCES PRIOR TO 1961. Edited by M. GERTRUDE HOWELL, ANDREW S. KENDE and JOHN S. WEBB. Pp. xiv + 206. New York: Plenum Press. 1965. $17.50. This volume contains literature references to the nuclear magnetic resonance spectra of over 2000 chemical compounds. Compounds are arranged in order of empirical molecular formula, but structural formulae (where known) are also included. Each compound is fully referenced for every occurrence noted in the literature. Despite the high price of the book, it can be recom- mended as a useful addition to the reference library of any chemistry department’s nuclear magnetic resonance spectroscopic service. K. G. ORRELL PKIXCIPLES OF REACTION KINETICS.By P. G. L 4 ~ ~ ~ ~ ~ ~ ~ , h1.,4. , Ph.D. h1onogvafihs f o v Teaclzevs, N o . IX. Pp. iv + 78. London: The Royal Institute of Chemistry. 1965. Price 7s. 6d. The series has been very helpful in general, although some of the volumes are “strong meat.” Dr. Ashmore has taken great trouble to make his exposition clear and lucid. His introductory survey covers the dissociation of simple molecules and the recombination of free atoms. The conccpt of activation energy is discussed in terms of the dissociation of bromine and the reaction between hydrogen and deuterium. The “transition complex” theory of Polanyi and Eyring is explained. Complex reactions are then discussed, and the difference between an intermediate species and a transition complex is emphasised.In Chapter I1 methods are given for the experimental measurements of rates, and the rate laws are established from these. Third- order reactions are treated in Chapter 111. Examples discussed include the hydrolysis of alkyl halides, the Harcourt and Esson reaction, the reaction between bromine and bromate ions, thermal clissociation of gases, reactions between ions in aqueous solutions, and reactions catalysed by surfaces. General reactions, for example, the photochemical hydrogenation of the halogens, are explained in Chapter IV, and a most useful ri.sum6 in Chapter V concludes the monograph. This latest addition to the R.I.C. Monographs for Teachers is most welconic. G. V.4x PRAAGH OPTICS, WAVES, ATOMS, AND WUCLEI: Ax INTRODUCTIOK. By EDWIX L. GOLDWASSER. Pp.xviii + 265. New York and Amsterdam: W. A. Benjamin Inc. 1965. Price (cloth) $6.60; (paper) 94.35. It is in tended primarily for undergraduate students in physics and engineering, and assumes: 3 familiarity with the principles of mechanics, electricity, heat and elementary calculus. The book starts with a brief but effective presentation of the fundamentals of the propagation of light and geometric optics. There follows a treatment of the properties of wave motion, which is developed through the study of waves in ropes, interference effects and resonant vibrations in sound and water waves, to the concept of light as a transverse electromagnetic wave disturbance and the phenomena of polarisation, interference and diffraction. A brief review of atomic structure and atomic spectra makes clear the failure of classical mechanics in atomic problems, and this leads on naturally to the consideration of the particle nature of light, the wave properties of matter, 1% ave mechanics, and finally nuclear structure and nuclear energy.The book thus provides a broad view of the relationships between radiation and matter, and will be of value to students of physics and chemistry alike. A surprisingly wide range of subject matter is collected within the scope of this book. C. A. PARKER MODLRX ~ L ~ E T H O U S 01; CHEMICAL ANALYSIS. By J. A. BARNARD and R. CHAYEN. Pp. xiv + 273. 1965. To anyone wishing to acquire a general introduction to a selection of relatively new, and some not-so-new analytical techniques, this book should have a special appeal.The six main headings are Volumetric Methods, Polarography, Spectroscopic Analysis, Mass Spectrometry, Radiochemical Methods and Separation Techniques, with a comprehensive list of references a t the end of each section. Almost half of the book, comprising the last section, deals with chromatography, ion exchange, gel filtration and zone electrophoresis. The book is primarily intended for students a t undergraduate level; it is easy to read and is well produced. G. WOLFENDEN London, New York, Toronto and Sydney : 1LIcGraw-Hill Publishing Company Ltd. Price 42s. 6d.January, 19661 BOOK REVIEWS 61 ADVANCES IN ANALYTICAL CHEMISTRY AND INSTRUMENTATION. Edited by CHARLES N. REILLEY. New York, London and Sydney: Interscience Publishers, a Volume 3 of this series was reviewed in The ,4nuZyst (1965, 90, 61) and the features of Volume 4 are similar to those of the preceding volume.This latest volume, like the earlier publications in this continuing series, contains contributions by universally recognised specialists. The subjects covered are : Recent Advances in Precipitation from Homogeneous Solution, Differential Dialysis, the Oxygen-flask Method, Phase-solubili ty Techniques, the Electrochemistry of Cation-scnsitivc Glass Electrodes, Recent Advances in Time-of-flight Mass Spectrometry, and Organic Analysis with Ultraviolet - Visible Absorption Spectroscopy; an additional index covers the four volumes now published. Volume 4 is up to the high technical standard of the earlier volumes, and the reviewer's favourable comments are equally applicable, including : “This is a book that the progressive analyst should read, but the price is likely to deter the average reader from wishing to make it a personal OXIDATION MECHANISM.By T. A. TURNEY, M.Sc.(N.Z.). Pp. viii + 208. London: Butterworth In this book, Turney gives an illustrated general account of oxidation mechanisms using as a framework a classification of reacting species rather than any of the conventional divisions of chemistry. After a brief introduction, there are chapters on cation - cation oxidations, cation - substrate oxidations, oxidations by cation-producing species, anion - anion, anion - complex and complex - complex oxidations, anion - substrate and complex - substrate oxidations, esterification- type oxidations, homolytic oxidation in solution, homogeneous oxidation in the gas phase, and heterogeneous oxidations.Each class is further subdivided as required and profusely illustrated by discussion of particular reactions. In this way, if a reaction is not specifically dealt with in the text, a pattern is provided that can be extrapolated to new situations. The coverage is com- prehensive for homogeneous reactions : for heterogeneous reactions, the treatment is restricted to reactions involving molecular oxygen, oxygen carriers, ozone and manganese dioxide, so that electrolytic and corrosion processes are excluded. The majority of the many references fall in the period 1950 to 1963 ; none is later, but important earlier studies are not neglected. The relevance of all this to analytical chemistry is not difficult to discover.Most of the reactions and reaction types considered are analytically important, and information on the actual pathway that the reactions follow cannot be other than valuable. A reaction, for example, that proceeds through the intermediate formation of a hydroxo complex cannot be expected to proceed in acidic media wherein the formation of the complex is inhibited, although the over-all reaction may involve neither hydrogen nor hydroxyl ion. In such conditions, the inhibiting effect of hydrogen ion may have been the subject of an empirical experimental observation, but the effect cannot be appre- ciated without a proper mechanistic investigation, nor can proper limits be placed on the experi- mental conditions in the analysis unless the situation has been investigated quantitatively, that is, by the determination of rate constants.The equilibrium situation and over-all stoicheiometry of a reaction afford essential information to the analyst, but do not completely define the situation, because the mechanism and speed of the processes leading to the final equilibrium often involve factors of even greater importance, and it is only by an appreciation of the total situation that the analyst can bring his processes completely under his control. Turney has provided a ready source of reference for a great many oxidation - reduction processes, in which each reaction is treated clearly, simply, non-mathematically yet quantitatively, in a .\l-ay that will be under- standable even by those with no detailccl knowledge of reaction kinetics.Argument is eschewed ; the author gives a simple statement of the current state of knowledge of each process, and if some points are debatable, the unsettled issues are unlikely to affect the application to analytical processes. I t is, however, most unfortunate that the author adhered to the old-fashioned American sign convention for electrode potentials. Certain other peculiarities of definition and of symbolism (not always consistent) also require an effort for assimilation, but a t the very reasonable price this is a book that should appear on the bench or desk of all analytical chemists. E. BISHOP THE CHEMISTRY OF THE RARE-EARTH ELEMENTS. By N. E. TOPP, Ph.D., F.R.I.C. Pp. xii + 164. Amsterdam, London and New E’ork : Elsevier Publishing Company.Dr. Topp’s death occurred before he had an opportunity of scrutinising the page proofs of this work. To quote the words of Professor P. L. Robinson, general editor of this series, “For a number Volume 4. division of John Wiley & Sons Inc. 1965. Price 120s. Pp. viii + 513. possession.” w. -r. ELWELL & Co. (Publishers) Ltd. 1965. Price 35s. 1965. Price 55s.62 BOOK REVIEWS [Analyst, Vol. 91 of years the rare-earth elements had been Dr. Topp’s major scientific preoccupation and perhaps this monograph is an appropriate memorial to a life too soon brought to a close.” Those who, like the reviewer, enjoyed the privilege of association with this gentle scientist with an acute mind will recognise his quiet authority in his writing and be grateful to the anonymous friends who have seen the text through the final stages.While paying due tribute to the heroic labours of the earlier workers in this field, the author addresses himself to the task of critically appraising the current state of knowledge of the chemistry of elements 57 to 71 and yttrium, largely on the basis of work initially stimulated by the occurrence of these elements in fission products and facilitated by modern separation and purification processes. The treatment is predominantly practical and is informed throughout by the author’s own experience. Of particular interest to analytical chemists are the chapters on separation methods-Topp’s special field of work-and analytical methods, which are excellent.The practical complexion lightens the emphasis on periodic relations within the group. For example, the contention that the solution chemistry of the ions is a function of increase in hydration of the ions with increasing atomic number is not argued in the text. However, as a clear, concise, up-to-date and authoritative account of the subject, this book will find a warm welcome from all who teach, read or practise in this field. E. BISHOP PERIODIC CORRELATIOKS. By RONALD RICH. Pp. xvi + 159. New York and Amsterdam: This is one of the volumes in the series of undergraduate texts presently being issued by Benjamins under the general title of “Physical Inorganic Chemistry.” All are available in the paper- back form convenient for students. The series emphasises the new systematic and fundamental approach to inorganic chemistry and is a valuable contribution to the literature. The present volume is one of the more provocative ones, and offers stimulative reading for the lecturer and the more intelligent undergraduate who is capable of weighing things up for himself.However, lecturers should hesitate to recommend it to the moderate or dull student without concurrent exposition, lest it confuse him. The series deals with the materials under daily requisition and examination by the analyst, and does so in a way that can only illuminate his understanding of them. The older chemist who came up through the old-fashioned inorganic and general chemistry grind, and who seeks to put himself in touch with the modern approach will find profitable, interesting and entertaining reading in this series of volumes, and in this one in particular, which are good and sound examples of the newer type of text-book.SCIENTIFIC REPORT No. 1. COLORIMETERS WITH FLOW-THROUGH CELLS. A CRITICAL ASSESSMENT OF FOUR INSTRUMENTS. Pp. 54. The Association of Clinical Biochemists. 1965. Price 13s. 6d. This report presents the results of a “which” hunt on four colorimeters fitted with “flow- through” cells such as are in popular demand for clinical testing in hospital laboratories. I t should be noted that “flow-through’’ does not mean a continuous flow of sample solution, but a cell that can be filled (by hand) and emptied (by suction) without having to remove the sample cell from the instrument. The instruments tested are the E.E.L.Flowthrough Spectra, the Gallenkamp Colorimeter, the Linson 3 Photometer (Swedish) and the Unicam SP1300 Colorinieter. Two samples of each instrument were examined, and showed surprising differences in certain respects. IT-ithin the terms of reference of the project (self-emptying cells and general applicability) the instrunients are comparable, but as colorimeters the E.E.L. is a stranger being provided with an interference-wedge dispersive element whereas the others are filter photometers. The E.E.L. colorimeter is instrumentally similar to the others tested, but the E.E.L. spectra is perhaps more comparable to the Uausch and Lomb Spectronic 20. However, the two testers have made a most thorough, competent, comprehensive and well planned job of the comparison and evaluation and have packed 50 pages with terse relevant and valuable information.Your reviewer has had to conduct “which” hunts of varying complexity and depth in collaboration with his colleagues into the whole gamut of items from corks, bark, to stills, pilot, and balances, rough, to spectro- meters, nuclear magnetic resonance, that go to equip a large research and teaching department, and his life would have been much simpler had reports of this nature been available. The contents of the report are worth recording: List of instruments tested (with prices and specifications); Description of the instruments (a comprehensive tabulation) ; Operation and critical testing of instruments-design and appearance, infinity optical-density setting, zero optical-density setting, galvanometer (and scales), the lamp, cell carriage, wavelength selection, reserve sensitivity, Unicam light-limiting stop ; Flow-through cells-critical evaluation of the different cells, possible W.A. Benjamin Inc. 1965. Price (cloth) $8.80; (paper) $4.35. E. BISHOPJanuary, 19661 BOOK REVIEWS 63 errors in the use of cylindrical cells, criticisms, features of a good flow-through cell; Photometric error ; Reproducibility ; Sensitivity and linearity-evaluated on oxyhaemoglobin, biuret protein, ammonia (Kessler), phenol, salicylate, summary ; Choice of reference solution ; Comparison of two samples of the same instrument ; Maintenance ; Instruction booklets (oh, when will manufacturers master the art of writing instructions ?) ; Faults developing during testing; Discussion and con- clusions ; Summary ; Modifications.This does not mention the considerable amount of wisdom and experience relevant to colorimetry and coloritneters in general that ornament the report and make it profitable reading for those who are not concerned with the primary question of “which ? ” Members of the Consumers’ Association will notice one omission-electrical safety. There is another-the “best buy.” However, with their own necds in mind, readers should have little difficulty in making this decision on the basis of the wealth of information provided. The constructive criticisms will, it is to be hoped, be duly notcd by manufacturers of photometric instruments to our future gain. E. BISHOP PRACTICAL CLINICAL ENZYMOLOGY.By J . KING. Pp. viji + 363. London, Frinceton (New ,4s one who worshipped devotedly a t the shrine of Organic Chemistry some significant fraction of a century ago, the reviewer tended to regard the biochemists’ numerous calls on enzymes to explain reactions as facile inventions to be treated with scepticism. But “tempora mutantur, nos et niutaniur in illis” and a closer contact with biochemistry in later years has dissipated the scepticism. In the last three or four decades the reality of enzymes has been reinforced by the multiplicity of their isolation and have not a number of them even been crystallised, which should satisfy the organic chemist ! ,4nd apart from being the bases of hypotheses they have become practical tools in the service of mankind, both in controlling the health of its body and to some degree also the wealth of its manufactures.This has inevitably brought enzymes within the ambit of the analytical chemist, though from this point of view, their involvement is mostly with the clinical chemist. For the analyst, there are two aspects of interest in enzymes-their determination and their use as reagents for the determination of substrates. This volume is restricted to the former and to the more common enzymes with clinical diagnostic value, but the methods, chosen on the basis of experience, naturally have a wider applicability. After initial lucid chapters on the nature and kinetics of enzyme activity in which the Inter- national Union of Biochemistry classification of enzymes is summarised, there follows a separate consideration of the measurement of enzyme activity, which, since enzyme reactions are reversible and tend to equilibrium mixtures unless the product is removed, forms a very useful background to the methods described in five subsequent chapters.The selectivity in these chapters will be understood when it is realised that the above classification includes 114 groups with as many as 50 enzymes in some groups. Actually, 31 enzymes are dealt with in detail, viz., 9 dehydrogenases, 6 transferases, 14 hydrolases, 1 lysase and 1 isomerase. Each chapter opens with a discussion of those characteristics of the group that have a bearing on the assay. Then follow the occurrence and characteristics of the reactions catalysed by certain specific enzymes and a general considera- tion of assay methods with a detailed description of the methods preferred.This is followed by the range of normal human values, the clinical interpretation of results and a bibliography. In most instances two methods of assay are described-a rate of reaction method followed spectro- photometrically, and a colorimetric method with a fixed period of reaction. The final chapter consists firstly of a review of the work, mostly of the last 6 or 7 years, on the heterogeneity of enzynics and secondly, of practical electrophoretic methods of separating the constituents of an enzyme. This gives point to the complexity of the problem of enzyme identity and consequently of its determination. Just as it was originally thought that vitamin activity belonged to a single unique substancc but was later found to be exhibited to varying degrees by related substances, so it has been shown that the same reaction can be catalysed by many enzymes on many substrates.Thus lactic acid dehydrogenase is separable into five components and unless these are separated, what is determined in an assay is not an amount of a specific substance but an amount of enzyme activity. This is a particularly valuable chapter in bringing out possible pitfalls in interpretation. For the clinical biochemist this volume is much more than a conipendium of methods; the methods are illumined by clear expositions of their raisons d’etre. Apart from a very few typo- graphical errors, the reviewer notes a reversal of captions to the graphs on p.51; and erroneous formulae for glucose-&phosphate (p. 56) and fumarate (Krebs cycle, p. 15). Jersey), Toronto and New York: D. Van Nostrand Company Ltd. 1965. Price 75s. The biochemists were right-possibly more so than they themselves believed. J. I. M. J o s ~ s64 BOOK REVIEWS [Analyst, Yol. 91 DIE KOMPLEXOMETRISCHE TITRATION. Fifth Edition. By DR. GEROLD SCHWARZENBACH and DR. HERMANN FLASCHKA. Pp. xvi + 339. Stuttgart: Ferdinand Enke Verlag. 1965. Price (cloth) DM 53; (paper) DM 48. The value of complexometric titration in modern inorganic analysis is well recognised, and the substances that were formerly known as Schwarzenbach’s complexes are now commonplace and have found a prominent place on most laboratory shelves. Although many analytical chemists in many countries have contributed to the development of the technique, few indeed have made such major contributions as the authors of this new, entirely re-written edition of Schwarzenbach’s original book on the topic.This text bears the stamp of the excellent blend of Schwarzenbach’s theory and Flaschka’s practicality, not that anyone would dispute that both authors also possess the complementary quality in full measure. The text presents a sweeping panoramic view of the theory and practice of the technique and reveals many new facets of the subject that will be of interest to most readers. In Part I, the introductory four sections treat the essential principles of titration with complex- forming substances, the nature of aminopolycarboxylic acids, the formation of complexes and their stability and the essential features of complexometric titration curves.The text then gets down t o business with detailed treatments of colorimetric and fluorimetric indicators and the reaction mechanism of metallochromic indicator functioning. The section on instrumental methods of end-point detection is full and detailed, although one notes with some amusement that even these distinguished authors make the student’s mistake of classifying coulometric titration (a technique of titration not using a burette) as an end-point detection method. An extensive survey is next given of titration techniques (direct-, back-, substitution, etc.) and, finally in this first part, a chapter on selectivity which deals with masking, demasking, indirect methods, etc.Part 11, consituting over 120 pages of the text, gives a monographic treatment of experimental procedures for each of over fifty metals and non-metals. The state of development of the technique is such that selected procedures of the authors’ choice only are given and most readers will be pleased to have such an authoritative and definitive review of procedures and recommendation of methods for individual metals and non-metals. Undoubtedly this book is of vital importance to all analytical chemists. It is a rare blend of theory and practice which can only enhance the reputation of analytical chemistry. English readers may be sorely tempted to buy this excellent German edition despite the fact that Professor Irving is understood to be preparing an English translation for publication in the near future. T.s. ~ ~ ‘ E S T The cost is moderate; the value is excellent. GRAVIMETRIC ANALYSIS. Part 11. By LASZLO ERDEY. Translated by GYULA SVEHLA. Edited by ILONA BUZAS. Pp. xvi + 796. Oxford, London, Edinburgh, New York, Paris and Frankfurt: Pergamon Press. 1965. 120s. This is an English translation of the original German edition previously reviewed in The Analyst, 1965, 90, 510. The sub-title of the former edition, “The Determination of Metals,” is missing from the title page and there are a few other other minor changes in the text, but none to warrant special mention. This is, as I have remarked before, a very worthwhile book, which can be recommended in the highest terms. It will undoubtedly receive very heavy usage in all laboratories where it is found.Once more it is necessary to report that the binding of this Perganion edition is very much inferior to the original Hungarian production. I t would appear to be a very short-sighted policy for the publishers to have put such an excellent and weighty text in so flimsy a spine. T. S. I \ r ~ ~ ~ ION EXCHANGE. By FRIEDRICH HELFFERICH. Pp. x + 624. New York, San Francisco, Toronto, Those who have not already obtained a copy of this book and are likely to make an extensive use or study of ion-exchange reactions, would be well advised to do so. It is a most useful source of information on the theoretical aspects of ion exchange, and has been translated from the original German by the author himself. In his preface the author mentions that there was some slight criticism of the German edition, in that practical chemists and chemical engineers found that the book required too great a background knowledge of mathematics and theoretical chemistry, whilst those who were interested in the theoretical aspects found that some of the explanations and London; McGraw-Hill Book Company Inc.1962. Price 136s.; $17.January, 19661 BOOK REVIEWS 65 of complex phenomena were too facile. As a result, Dr. Helfferich has now separated the quali- tative and quantitative treatments more sharply than in the original edition. The mathematically disinclined reader may now omit all mathematical equations and deductions without loss of continuity. The result is not entirely satisfactory, however. The main part of the text still covers too wide a range of theoretical aspects (even though these are not treated in great depth), without providing sufficient details of practical operation and application to satisfy those interested primarily in the use of ion exchangers.Those who are more concerned with the theoretical aspects of ion exchange will find that the more theoretical sections in smaller type taken on their own do not necessarily give them all the information that they require. They will have to consult the sections in larger type as well, only to find, in addition, a change from a precise to a more superficial style of presentation. It is therefore, unfortunately, not a book that is easy to read, but, for the research worker it is a valuable source of information on the properties of ion-exchange materials, and the theoretical aspects of ion-exchange systems.It is to be hoped that, if future editions are being considered, the author will concentrate on presenting the theoretical aspects of ion exchange in a more uniform style. Those whose interest in ion exchange is relatively slight and of a strictly practical nature would be better advised to consult other shorter monographs that are directly aimed at their needs. The book is divided into twelve chapters of which the first four deal with the more practical aspects of ion exchange. These chapters are entitled : Elementary Principles, Structure and Properties of Ion Exchangers, Preparation, and Capacity. The division into two levels of approach referred to above has been kept to a minimum here, and as a consequence these are the most readable chapters of the whole book.Since this part could be read with profit by the beginner, it is unfortunate that in the section on Mineral Ion Exchangers in Chapter 2, the reader could be misled into believing that the ionic sieve effect and the niolecular-sieve properties of zeolites were one and the same thing. The fifth, sixth and seventh chapters deal with fundamental properties of ion-exchange systems, and are entitled : Equilibria, Kinetics and Electrochemical Properties, respectively. I t is these chapters that would benefit most by a more uniform style of presentation. The eighth chapter deals with the special characteristics of ion-exchange membranes, whilst in chapters nine and ten, dealing with Ion-exchange Columns and Behaviour in Nonaqueous and Mixed Solvents, respectively, there is a return to a more practical aspect of ion exchange, but the approach is still largely theoretical, and the reader will look in vain for details of operation.The last two chapters deal with the more specialised subjects of Catalysis by Ion Exchangers, and with Electron Exchangers and Redox Ion Exchangers, respectively. Each chapter has a fairly extensive list of references amounting sometimes to well over 200 entries, and these can easily be supplemented and brought up to date by annual reviews published on ion exchange and from other sources. There are three useful appendices and an author and subject index. There is no doubt that Dr.Helfferich’s knowledge of the field is exten- sive, as is indicated by his many contributions to it. He has done a useful job for the research worker, and the only criticism of the book is really that he is trying to satisfy both the advanced research worker and the beginner in the field a t the same time. J. E. SALMON KIRK-OTHMER ENCYCLOPEDIA OF CHEMICAL TECHNOLOGY. Volume 5. CHLORINE TO COLORS FOR FOODS, DRUGS, AND COSMETICS. Edited by HERMAN F. MARK, JOHN J . MCKETTA, jun., DONALD F. OTHMER and ANTHONY STANDEN. Second Edition. Pp. xiv + 884. New York, London and Sydney: Interscience Publishers, a division of John Wley & Sons Inc. 1964. Price Ll6 18s. ; price per volume for subscribers to the complete set of 18 volumes k13. The fifth volume of this encyclopedia follows the general pattern that is starting to emerge, following the publication of its predecessors (see Analyst, 1963, 88, 899; 1964, 89, 502, 752; 1966, 90, 375).It has, however, certain distinguishing features that will appeal to British readers and to analysts in particular. The former will be glad to find more contributions from British authors than have occurred in previous volumes, because these reflect the practice and current opinions on this side of the Atlantic. Thus, Shell Development Company and Imperial Chemical Industries Ltd., have provided contributors dealing with chlorocarbons and chlorohydrocarbons ; and Dr. R. D. Powell of Cadbury Brothers Ltd., deals with chocolate and cocoa. Analysts will welcome the rather more detailed and frequent analytical sections that occur in some of the present articles; further reference is made to certain of these below.Whether the above two features are accidental and peculiar to this volume only, it is not possible to say, but to the present reviewer they give i t an enhanced value.66 BOOK REVIEWS [Analyst, Vol. 91 C is an important initial letter in the chemical alphabet and consequently there are several long articles in this volume. Chlorine (the manufacture of which was dealt with in Volume 1, under Alkali and Chlorine Industries) together with its oxyacids, salts, carbon tetrachloride, chlorohydrin and chlorophenols, occupies 338 pages, i.e., nearly 40 per cent. of the volume; it is therefore possible to give full treatment to the subject in a space of this magnitude, and full advantage has been taken. Coal accounts for a further 72 pages, and the various ramifications of colour (colour and constitution of organic dyes, colorimetry, colour measurement, colour photo- graphy and food, drug and ceramic colours) occupy a further 120 pages. The article on chlorophyll may, perhaps, be singled out for comment as of special importance, because it also covers compounds such as the rhodins and chlorins, about which there is a dearth of readily available, published information. Its scope and modernity of treatment are evident from the fact that it deals with deodorising (described as “a multifaceted and growing, yet contro- versial field of application”) ; and food for space travel (interesting but speculative, since it refers to the, as yet unsccomplished, feat of reducing carbon dioxide with extracted chlorophylls).Analysis receives 2 pages, in the course of which it is stated that in every commercial sample examined by the author, part of the copper content was present as the Cu2+ ion, which could be separated by dialysis and determined electrolytically. Chocolate and cocoa are the subject of an excellent article (40 pages) treated with a marked manufacturing bias. There is a section on quality control in which the pH value is recommended as a method for evaluating the degree of alkalisation; however, in certain circumstances this method can prove unreliable. Chromatography is dcalt with in approximately 40 pages, and analysts will find this article useful as an introduction, particularly to the theory of the subject.However, it is developing so rapidly that most workers will probably prefer the more practical monographs that have been published in recent years. The principal methods are described briefly, including thin-layer methods, but naturally gas - liquid chromatography receives the most attention. Chromium and its compounds are dealt with in 63 pages. An article on clays is sub-divided into Survey and Uses, the former being mainly mineralogical and geological in character. The latter includes a number of important industries, ranging from bricks to catalysts and radioactive waste disposal. The use of kaolin to improve the quality of paper receives due attention, though, its economically more important use in the paper industry, namely as a filler to cheapen the production cost, is not mentioned. Two successive articles deal with Coated Fabrics and Coatings Industrial : another example of the somewhat indiscriminate alphabetical use in this work of adjectives and nouns. The former covers rubber compounds, cellulose derivatives and vinyl compounds, and briefly describes the impregnation and surface methods. The procedure is so similar to that used for paper coating that the two could have been covered together, especially as the latter is dealt with in Coating Industrial superficially, the reader being referred to Paper Converting. Coffee takes 15 pages, most of which refer to instant coffee and decaffeinated coffee, signs of the times, indeed. The economics, technology and chemistry of the subject are summarised usefully, and there is an imposing table of some 60 chemical compounds that have been detected in coffee aroma ; surprisingly, they include carbon disulphide, mercaptans, and phenols. The section on colorimetry includes fluorimetry, and again, the treatment tends to be on the theoretical side, analytical methods being referred to through the bibliography, though not dealt with in detail. Analysts will, nevertheless, find this article a useful, if brief, survey of the funda- mentals of the subject. Colour measurement is discussed in a separate article and is followed by Color Photography, Colors for Ceramics and Colors for Foods, Drugs and Cosmetics (83 pages in all). The last article is based wholly on the F.D. & C. regulations; these are given and discussed in detail. All the currently listed, certified colours are tabulated, with their chemical and trade names, manufacturing process, shade, uses, solubilities and fastness data. As the Colour Index reference numbers are also included, this should prove useful to chemists in other countries, particularly in Britain. It is once again apparcnt that this volume maintains the high standard of those issued previously and, if anything, has rather more to offer the analyst than some of its predecessors. I t may be recommended with confidence and in the same terms as those of the earlier reviews. JULIUS GRANT

ISSN:0003-2654    

DOI:10.1039/AN9669100057

出版商:RSC    

年代:1966

数据来源: RSC

摘要:

January, 19661 NOTICE TO AUTHORS 67 Notice to Authors THE Society publishes papers on all aspects of the theory and practice of analytical chemistry] fundamental and applied, inorganic and organic, including chemical, physical and biological methods. Such papers may describe original work or may present in review form a critical evaluation of the existing state of knowledge on a particular facet of analytical chemistry. Papers may be submitted for publication by members of the Society or by non-members. Papers and all correspondence relating thereto should be sent to the Editor of The Analyst, 14 Belgrave Square, London, S.W.l. Every paper will be submitted to a t least two referees, by whose advice the Editorial Committee of The Analyst will be guided as t o its acceptance or rejection.Papers that are accepted must not be published elsewhere except by permission of the Committee. Submission of a manuscript will be regarded as an undertaking that the same material is not being considered for publication by another journal. Manuscript.-Papers should be typewritten in double spacing on one side only of the paper. Three copies (top and two carbon copies) should be sent to the Editor, and a further copy retained by the author. Title and synopsis-The title should be brief but descriptive, and must pin-point the original features of the work. All papers must be accompanied by a short synopsis of about 100 to 250 words; this should give the principle of the method, draw attention to its novel features and indicate its scope and sensitivity. Contributions t o the Short Papers section do not require synopses.Pvoofs-The address to which proofs are to be sent should accompany the paper. Proofs should be carefully checked and returned within 48 hours of receipt. Reprints-Twenty-five reprints, or a maximum of fifty if there is more than one author, are supplied gratis. Additional reprints may be obtained a t cost if ordered directly from the printers, W. Heffer & Sons Ltd., Hills Road, Cambridge, at the time of publication. Details are sent t o authors with the proofs. NOTES ON THE WRITING OF PAPERS FOR The Analyst Manuscripts should be in accordance with the style and usages shown in recent copies of Conciseness of expression should be aimed a t : clarity is increased by adopting a Descriptions of new methods should be supported by experimental results showing accuracy, The recommended order of presentation is as indicated below- (a) Synopsis.(b) The A naZ*yst.* logical order of presentation] with suitable paragraph or section headings. precision and selectivity. Statement of object of investigation and, if necessary, historical introduction and account of preliminary experimental work; these need be no longer than is necessary for the understanding of the new material. (c) Description of method. When working details are given, they should, if possible, be given in the imperative mood. (d) Presentation of results. (e) Statistical analysis of results. Any statistical evaluation of results should be in accordance with accepted practice. (f) Discussion of scope and validity. (g) Summary and conclusions.Tables, diagrams, etc.-The number of tables should be kept to a minimum. Well known procedures must not be described in detail. Column headings No Tables must be supplied with titles and be so should be brief. lines should be ruled in tables in the manuscript. set out as to be understandable without reference to the text. Chemical Society, Rurlington House, London, W. 1) are followed. is followed for spelling, but some words are given that Dictionary’s secondary alternative spelling. Tables consisting of only two columns may often be arranged horizontally. * Rules for nomenclature in “Handbook for Chemical Society Authors 1961” (price 21s. from the The Shorter Oxford English Dictionary68 NOTICE TO AUTHORS [Analyst, VOl.91 Tables or graphs may be used, but not both for the same set of results, unless important additional information is given by so doing. In general, graphs should have a reasonable number of co-ordinate lines, and not only the two main axes. The information given by a straight-line calibration graph can usually be conveyed adequately as an equation in the text. Diagrams and graphs should be drawn in Indian ink on Bristol board, stout paper or tracing cloth, not larger than foolscap size and with a t least 1-inch margins all round. The use of squared paper should be avoided. All lettering should be inserted lightly in black lead pencil a t the appropriate place in the diagram, and will be replaced by type in block-making. All lines in Indian ink should be firmly drawn and sufficiently thick to stand reduction.Drawings should be specially prepared for submission to The Analyst, as they cannot normally be returned and may be modified or cut in the course of block-making. Three sets of illustrations should be provided, two sets of which may be photographic or dyeline copies of the originals, or pencil sketches, for transmission to the referee; there is no need to prepare Indian-ink duplicates. Photographs-Photographs should only be submitted if they convey essential information that cannot be shown in any other way. They should be submitted as glossy prints made to give the maximum detail. Colour photographs can only be accepted when a black-and-white photograph fails to show some vital feature. A bhveviations-Normality and molarity are generally expressed as decimal fractions (e.g., 0.02 N , 0.375 M).Abbreviational full stops are omitted after the common contractions of metric units (e.g., ml, g, pg, mm) and after “C, O F , p, A and other units represented by symbols; litre and metre, when without prefixes, are printed in full. Abbreviations other than those of recognised units should be avoided in the text; symbols and formulae are not used instead of the names of elements and compounds in the text, but may be used in addition to names when they are necessary to avoid ambiguity, e.g., to specify crystalline composition, as in CuS0,.5H20, to show structure or in equations. Percentage concentrations of solutions should be stated as “per cent. w/w” (alternatively “g per 100 g”), as “per cent.w/v” (alternatively “g per 100 ml”) or as “per cent. v/v.” Concen- trations of solutions of the common acids, however, are often conveniently given as dilutions of the concentrated acids, such as “diluted hydrochloric acid (1 + 4),” which signifies 1 volume of the concentrated acid mixed with 4 volumes of water. This avoids the ambiguity of 1 : 4, which might be equivalent to either 1 + 4 or 1 + 3. Refevences-References should be numbered serially in the text by means of superscript figures, e.g., Mackenzie and Mitchell‘ or Furman,2 and collected in numerical order under “REFERENCES” and the end of the paper. They should be listed, with the authors’ initials, in the following form (double-spaced typing)- 1. 2. Mackenzie, R. C., and Mitchell, B. D., Analyst, 1962, 87, 420. Furman, N. H., Editov, “Standard Methods of Chemical Analysis,” Sixth Edition, D. Van For books, the edition (if not the first), the publisher and the place and date of publication should be given, followed by the volume or page number, or both if required. The entry of “personal communications” in the reference list is not justified; full acknowledg- ment of such unpublished sources should be made in the text or in the acknowledgments a t the end of the paper. Authors must, in their own interest, check their lists of references against the original papers; second-hand references are a frequent source of error, The number of references must be kept to a minimum. Nostrand Co. Inc., New York and London, 1962, Volume 1, p. 863.

ISSN:0003-2654    

DOI:10.1039/AN9669100067

出版商:RSC    

年代:1966

数据来源: RSC