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196 Analyst, March, 1967, Vol. 92, $9. 196-197 The Use of Iron (11) Sulphate for the Reduction of Nitrate to Ammonia in the Microdiffusion Method for Determining Nitrate in Soil Extracts BY P. R. PREMI AND A. €3. CORNFIELD (Chemistry Department, Imperial College of Science and Technology, London, S. W.7) Because of the variable nature of technical titanium(II1) sulphate normally used for the determination of nitrate in soil extracts by the Brem- ner - Shaw microdiffusion method, the possibility of replacing this reagent with iron(I1) sulphate was studied. It was found that 1 ml of M iron(I1) sulphate (in 0.5 M sulphuric acid) plus 0.1 ml of saturated silver sulphate could be used t o successfully determine up to 200 pg of nitrate nitrogen in 5-ml aliquots of soil extracts. THE use of titanium(II1) sulphate with magnesium hydroxide suspension for the simultaneous reduction of nitrate, and its determination as ammonia in soil extracts when using a micro- diffusion method, has been described by Bremner and Shaw.l Bremner2 developed the method by using steam-distillation instead of microdiffusion to drive off the ammonia.The technical titanium(II1) sulphate solutions available often give high blank values for ammonia and tend to lose their nitrate-reducing ability, even when stored in a refrigerator. Bremner and Shaw3 found that nitrate was quantitatively reduced to ammonia during steam-distillation with iron( 11) hydroxide (iron(I1) sulphate with excess of magnesium hydroxide), providing the iron(I1) concentration in the distillation flask exceeded 7 g per litre.Steam-distillation with alkali may cause hydrolysis of organic nitrogenous compounds usually present in soil extracts, thus giving high values for ammonia and also for nitrate, when this is being determined simultaneously by reduction. Because of this, the ability of iron(I1) hydroxide to reduce nitrate to ammonia at room temperature in the Bremner - Shaw microdiffusion cells was studied. EXPERIMENTAL Preliminary tests were made with pure nitrate solutions by using various concentrations of added iron( 11) sulphate (analytical-reagent grade) and excess of light magnesium oxide suspensions. When 5 ml of nitrate solution, 1 ml of M iron(I1) sulphate (in 0-5 M sulphuric acid) and 3 ml of 12 per cent. w/v light magnesium oxide suspension were used in the outer chamber, there was always complete recovery of up to 100 pg, but not of 200 pg, of nitrate nitrogen as ammonia in the central chamber when using the normal 48-hour diffusion period.The use of 2 ml, instead of 1 ml, of M iron(I1) sulphate sometimes gave incomplete recovery of even 100 pg of nitrate nitrogen, presumably owing to the restriction of diffusion of am- monia through the immobile gel of iron and magnesium hydroxides. However, it was found that the use of a silver catalyst4 increased the amount of nitrate that could be recovered as ammonia, even when using 1 ml of M iron(I1) sulphate. The use of 1 ml of M iron(I1) sulphate, 0.1 ml of saturated silver sulphate solution and 3 ml of 12 per cent. w/v light magnesium oxide suspension always gave complete recovery of up to 200 pg of nitrate nitrogen from 5-ml aliquots of test solution. It is worth noting that the minimum concen- tration of iron(I1) sulphate required in the outer chamber for complete recovery of nitrate as ammonia is similar to that required in the distillation flask when using steam-distillation.3 The method was then tested on extracts of several soils.The extracting reagents used were (i) N sodium chloride and (ii) the “Morgan reagent” (0.5 N acetic acid - 0-75 N sodium acetate, pH 4.8). Ten grams of air-dried, 2-mm sieved soil were shaken with 20 ml of extracting reagent for various times and filtered. When using 5 ml of the extracts, the results obtained with iron(I1) sulphate plus silver sulphate were almost identical with those obtained with titanium(II1) sulphate (ammonia present was allowed for after determination on a separate aliquot by reaction with light magnesium oxide suspension).Both methods also gave 100 per cent, recovery of known amounts of nitrate nitrogen added to the extracts. When an un- usually high amount of nitrate or ammonia, or both, is present in an extract, necessitatingPREMI AND CORNFIELD 197 the use of an aliquot of less than 5 ml, water should be added to the outer chamber to dilute the aliquot to 5ml before adding the other reagents. CONCLUSIONS One millilitre of M iron(I1) sulphate (in 0.5 M sulphuric acid) $ h s 0.1 ml of saturated silver sulphate can be used instead of titanium(II1) sulphate for the determination of up to 200 pg of nitrate nitrogen in 5-ml aliquots of soil extracts by using the Bremner - Shaw micro- diffusion cells. Iron(I1) sulphate has the following advantages over technical titanium(II1) sulphate: it is of constant quality; it is stable for at least 2 months when kept in a well stoppered bottle at 2” to 4” C; and it gives a low blank value for ammonia. REFERENCES 1. 2. 3. 4. Bremner, J. M., and Shaw, K., J . Agric. Sci. Camb. 1955, 46, 320. Bremner, J. M., “Rothamsted Experimental Station Report for 1959,” 1960, p. 59. Bremner, J. M., and Shaw, K., Analyst, 1955, 80, 626, Cotte, J., and Kahane, E., Bull. SOC. Chivn. Fr., 1946, 542. Received June 22nd, 1966

ISSN:0003-2654    

DOI:10.1039/AN9679200196

出版商:RSC    

年代:1967

数据来源: RSC

摘要:

198 Analyst, March, 1967, Vol. 92, p . 198 A Simple, Rapid Method for Determining Glucose in Blood or Plasma BY J. D. PRYCE HULTMAN~ studied the reaction between sugars and aromatic amines, which yields coloured azomethines. Hyverinan and Nikkila2 devised a method for determining glucose in blood by using orthotoluidine and stabilising the reagent by adding thiourea ; the present note describes a modification of their method, with a further simplification when applied to plasma. Dubowski3 has reported on the specificity of the method; the reaction involves the aldehyde group, and other reducing substances do not interfere. Although other sugars react, they either do so to a lesser extent, or absorb a t a different wavelength; in the absence of galactose the method can be regarded as virtually specific for glucose when applied to blood or plasma, and it gives about the same range of normal values as the enzyme methods, or the more specific of the copper methods.EXPERIMENTAL REAGENTS- solution well, and allow to settle. (Pathological Laboratory, Ipswich and East Suffolk Hospital, Anglesea Road, Ipswich) Methanol - thiourea-Saturate 100 ml of methanol by adding 10 g of thiourea; shake the Orthotoluidine. Glacial acetic acid, AnalaR. Colour Yeagent-Dilute 30 ml of saturated thiourea solution and 60 ml of orthotoluidine to 1 litre with glacial acetic acid. Prepare the solution 24 hours before use; the reagent can be dispensed from a “Zipette” (Jencons). Glucose solution-Dissolve 50, 100 and 250 mg of dried glucose in saturated benzoic acid solu- tion and make each solution up to 100 ml with the benzoic acid solution. Trichloroacetic acid-Dissolve 3 g of trichloroacetic acid in 100 ml of water. It is stable for a t least 2 weeks a t room temperature.PROCEDURE- Plasma-Separate plasma from blood preserved with fluoride by lightly spinning the mix- ture in a centrifuge for 2 to 3 minutes. If the specimen is grossly haemolysed, treat it as for whole blood. Place 4 ml of the colour reagent in a series of tubes (6 x + inches). Add 0.05 ml of plasma or standard (with no addition for the blank), mix, place in a boiling water bath for 5 minutes, then cool the solution. Measure the optical density a t 640 mp within 30 minutes; calculate the glucose content by proportion. Whole blood-Place 1.5 ml of 3 per cent.trichloroacetic acid in a centrifuge tube; add 0.1 ml of whole blood, or 0.1 ml of standard. Mix the solutions and spin them in a centrifuge for 5 minutes a t about 1500 r.c,f. Place 4 ml of colour reagent in a tube (6 x # inches), add 1 ml of supernatant liquid and mix; heat in a boiling water bath for 5 minutes, and measure the optical density at 640 mp within 30 minutes; calculate the glucose content by proportion. The extra water in the second procedure diminishes the colour yield, so the standards read lower. The methods have been in trouble-free use for over 1 year. The reaction does not appear to measure some hexose - phosphates, therefore stored fluoride blood may give low values on the red cell fraction. High colours can be measured by diluting with a further 4 ml of reagent, with no extra heating; the readings were linear up to 1000 mg per 100 ml. NORMAL VALUES- The mean and standard deviation for this method are as follows- 102 & 13.5 mg; and females, random: 119 f 19 mg. Plasma-Males, fasting: 101 * 12 mg; males, random: 129 * 13 mg; females, fasting: Whole blood-Males, fasting: 91 f 12 mg; males, random: 118 13 mg; females, fasting: 92 & 13.5mg; and females, random: 108 f 19mg. I thank the Research Committee of the East Anglian Regional Hospital Board for the REFERENCES of a printing calculator in connection with the statistical work involved. 1. Hultman, E., Nature, 1959, 183, 108. 2. 3. Dubowski, I(. M., Clin. Chenz., 1962, 8, 215. Hyverinan, A., and Nikkila, E., Clin. Chim. Acta, 1962, 7, 140. Received September 21st, use 966

ISSN:0003-2654    

DOI:10.1039/AN9679200198

出版商:RSC    

年代:1967

数据来源: RSC

摘要:

Analyst, March, 1967, Vol. 92,p. 199 199 An All-plastic Suction Funnel BY D. T. PRITCHARD (Soil Survey of England G. Wales, Rothamsted Experimental Station, Harpenden, Herts.) FOR the gravimetric determination of silica as potassium silicofluoride i t was necessary to collect the precipitate in apparatus unaffected by hydrofluoric acid. A suitable funnel, in which some of the disadvantages of normal filtration apparatus are avoided, was cheaply and easily constructed by using the upper half and the cap of a polypropylene bottle. Holes (1 to 2 mm in diameter) were bored in the top of the cap, and a disc of porvic" (0.75-mm * Porvic is a permeable material of fine and uniform porosity made from poly(viny1 chloride); Grade Available from Porous Plastics Ltd., Dagenham Dock, M has a pore size of 5p and Grade S of 12p.Dagenham, Essex.200 PRITCHARD [APzalyst, VOl. 92 thick) was cut to fit closely the inside of the holed surface. The cap was screwed into position on the upper half of the bottle locking the porvic disc between the cap and the top of the neck. The funnel was used with a Buchner flask and a conventional adaptor. To eliminate the problem of static electricity associated with the weighing of plastic materials a hygrostat was used instead of a desiccator. Precipitates do not seep under the porvic disc, and when the disc is wetted before filtration no supernatant liquid is held against washing in the periphery of the disc. Chemicals that attack glass can be used, and cleaning is simplified by replacing the porvic disc. 4 --3.5 cm- Fig. 1. Details of the funnel The funnel, illustrated in Fig. 1, weighs 8 g and has an effective filter area of 5-7 om2. To check thermal stability a funnel fitted with a porvic disc was heated at 60” C for varying lengths of time up t o 16 hours, and then weighed after standing in a hygrostat at 75 per cent. relative humidity for 1 hour. For gravimetry the drying temperature is restricted to 60” C, but many gravimetric precipitates can be dried to constant weight at, or below, this temperature1; porous Teflon with a funnel of Teflon or fluorinated ethylene - propylene would allow higher temperatures to be used. REFERENCE The maximum change in weight was 40pg. 1. Duval, C., “Inorganic Thermogravimetric Analysis,’’ Second Edition, Elsevier Publishing Co. Inc., Received July 22nd, 1966 Amsterdam, London and New York, 1963.

ISSN:0003-2654    

DOI:10.1039/AN967920199b

出版商:RSC    

年代:1967

数据来源: RSC

摘要:

200 PRITCHARD [APzalyst, VOl. 92 Effect of Impurity in Dichloroethane Solvent on the Determination of Boron with Methylene Blue BY A. STRIZOVIC AND J. A. CALDWELL (Research Department, Murex Ltd., Rainham, Essex) DURING an investigation into the spectrophotometric determination of boron in niobium oxide, an attempt was made to extract the fluoroborate - methylene blue complex by using a technique based on published work1 devised for the determination of boron in steel. After certain preliminary difficulties had been overcome an accurate and precise method was developed, but this subsequently appeared to give incomplete recovery of boron when applied by another analyst, The errors were traced to a batch of dichloroethane, which presumably contained an impurity that decreased the solubility of the boron complex a t the solven t-extraction stage. If viewed through a sufficient depth of solvent (about 2 inches) a slightly yellowish tint could be detected in the impure solvent. The effectiveness of the solvent was restored by washing it with small portions of sodium hydroxide, until the latter was colourless. Excess of alkali was removed by washing with dilute sulphuric acid and then water. REFERENCE 1. Pasztor, L., Bove, J. D., and Fernando, Q., Analyt. Chem., 1960, 32, 277. Received January 13th, 1967

ISSN:0003-2654    

DOI:10.1039/AN9679200200

出版商:RSC    

年代:1967

数据来源: RSC

摘要:

March, 19671 BOOK REVIEWS 201 Book Reviews STANDARD METHODS OF CHEMICAL ANALYSIS. Sixth Edition. Volume 111-Instrumental Methods, Parts A and B. Edited by FRANK J. WELCHER, Ph.D. Pp. xviii + 973 (Part A) ; Pp. xii + 2018 (Part B). Princeton, New Jersey, Toronto, London and New York: D. Van Nostrand Co. Inc. 1966. Price single volume A18 18s. If part of complete set A16 16s. The extent to which analytical chemistry has expanded since “Scott” made its first appearance in 1917 is shown by the size of this present edition, which now comprises five books, over 6000 pages, and literally hundreds of diagrams. Originally, the publication aimed at providing analytical chemists, irrespective of their specialised interests, with a collection of methods that had been well tried and authoritatively approved, hence in previous editions, and also in Volumes I and I1 of this edition, methods are regarded as standard if they meet this criterion. Over the intervening half century, analytical chemistry has undergone radical changes, its scope and importance have increased, and the field of chemical analysis has become even more specialised.To keep pace with these changes, and to continue to provide the analyst with a reliable source of collated information, it is understandable that the prime objective of “Standard Methods of Chemical Analysis” has been extended to include instrumental methods, many of which do not meet the earlier requirements of a standard method. This clearly recognises the present-day importance and potential usefulness of instrumental techniques, and the ever-growing importance of instrumental analysis, in its current context, in all branches of analysis.It is logical, therefore, and timely with the appearance of these two volumes, that an authenticated appraisal of established instrumental analytical procedures should be made available to the analyst, so that standard methods may be supplemented, if not replaced, a t his discretion. Part 1 of Volume IIIA contains forty-three chapters devoted to such subjects as Visible, Ultraviolet, Infrared, Raman, Atomic Absorption, and Emission Spectrometry, Electron Micro- scopy, Potentiometric, Amperometric and Conductometric Titrations, Coulometric and High- frequency Methods, . . . Particle Size Analysis. Each of the chapters is covered in comprehensive detail, and, like the other chapters in these volumes, all were prepared by experts in their specialised fields.The remaining five chapters of Volume IIIA (Part 11) deal with Instrumental Methods for Industrial Products and Other Special Substances, under the headings, Air Pollutants, Alloys : Iron, Steel, Ferro-Alloys and Related Products, Alloys ; Nonferrous, Amino Acid Analysis and Portland Cement. In Volume IIIB, the application of instrumental methods of analysis to Clinical Medicine, Natural Fats, Fertilizers, Foods, Organic Functional Groups, Glass, Paint, Varnish and Lacquers, Paper, Wood and Pulp, Pesticide Residues, Petroleum, Plastics, Rubber, Semi-Conductors, Detergents, Soils, and Water is described. Naturally, with each chapter written by a different author, the treatment is somewhat varied, but this in no way detracts from their value.Some chapters are fairly comprehensive compilations of official or near-official methods ; others are personal selections of non-standard methods that are in day-to-day use, and, in some respects, these have a special value. In total, these two volumes are an impressive accumulation of information, which the good indexing makes readily available. With the publication of these two volumes, the sixth edition of this book is complete. It must surely rest within the grasp of every analyst, to be turned to like a good friend, for confirmation of one’s own thoughts, for advice-or at times in sheer desperation! W. T. ELWELL J. F. HERRINGSHAW ANALYTICAL CHEMISTRY OF COBALT.By I. V. PYATNITSKII. Pp. xvi + 224. Jerusalem: Israel Program for Scientific Translations. Distributed in Great Britain and the Commonwealth, South Africa, Eire and Europe by the Oldbourne Press, London. 1966. Price 87s. 6d, Like previous monographs in this series, some of which have been reviewed in The Analyst, this is a translation of the original publication by the Institute of Geochemistry and Analytical Chemistry, U.S.S.R., and already about twelve of the series have either been translated, or are in the process of being translated, for publication in English.202 BOOK REVIEWS [Analyst, VOl. 92 These monographs on the analytical chemistry of individual elements will vary in their appeal, depending on the needs of the individual, but more especially on the availability of similar current publications.For this reason only, it is doubtful whether this latest monograph will have the same appeal outside the U.S.S.R. as the earlier members of the series, because of the recent appearance of an English publication under precisely the same title. (Reviewed in Analyst, 1966, 91, 754.) It would be improper to compare the relative merits of these two books here, but clearly, the contents of each overlap considerably. This book is devoted almost exclusively to the known chemical reactions of cobalt up to 1963. In addition to nearly 400 Russian references, it contains over 1000 non-Russian references, but of these, a rough assessment indicates that only about half are readily accessible to the average reader. The book provides a comprehensive coverage of the subject within its declared objectives, e.g., it does not claim to cover spectroscopic or X-ray analytical procedures, although some spectro- scopic methods are given; one chapter (4 pages) is allocated to polarographic methods, and radio- activation methods are dealt with in six paragraphs.This latest release provides a good companion to the earlier publications in the series. w. *r. ELWELL ALFRED WERNER FOUNDER OF COORDINATION CHEMISTRY. By GEORGE B. KAUFFMAN. Pp. xvi Not so many years have elapsed since historical chemistry formed an integral and compulsory part of many degree courses. Students were enjoined to read some of the memorial lectures of the Chemical Society dealing with the lives and achievements of such early pioneers as Liebig, Avogadro or Baeyer. If such a stipulation still prevails, the present volume on Alfred Werner deserves to be included among the books for recommended reading.Having said this, despite a contrary statement by the author, it is unlikely to appeal to the general reader who has no particular interest in the stereochemistry of co-ordination compounds. The author preserves a good balance between the biographical and scientific aspects of Werner’s life, and makes no attempt to ignore his human failings. Thus there emerges a portrait of “der grosse Mann,” the good-natured victim of buffoonery on social occasions but a stern task- master in the laboratory. As he gave of his utmost himself so he expected the same of others, and obviously did not suffer fools gladly.The various phases in the emergence of the co-ordination theory as developed by Werner are well described, culminating in the optical resolution of a purely inorganic compound and the award of the Nobel Prize in 1913. Professor Kauffmann rightly stresses the importance of Werner’s “Lehrbuch der Stereochemie,” and his interest in the development of stereochemistry during his lifetime. This provided much of the basis for his conceptions of molecular structure, which were mainly intuitively conceived and, a t best, of a semi-quantitative nature. Similarly, in his laboratory work, the simplest of equipment was used to produce the finest crystalline products, recalling the use of tannin by Dr. Schoeller in the analysis of mixtures of tantalum and niobium pentoxides.To sum up, the book is well produced, and includes an extensive bibliography, a good index, and a particularly fine set of photographs illustrating the work of the master and his pupils. The price is not excessive as judged by present-day standards. + 127. Berlin, Heidelberg and New York: Springer-Verlag. 1966. Price DM 24. F. G. ANGELL THE PHASE RULE. By F. D. FERGUSON, BSc., A.R.I.C., A.M.I.CHEM.E., and T. K. JONES, M.Sc., A.R.I.C. Pp. viii + 112. London: Butterworth & Co. (Publishers) Ltd. 1966. Price 15s. This is a very useful little book, especially for students a t the Higher National Certificate, Part I G.R.I.C., and Pass Degree levels. It deals with the essentials of the subject in a compact and readable form, and in many places gets away from the rather hackneyed examples that one all too often encounters in treatments of the phase rule.It covers one-component systems, two-component systems (liquid - liquid, liquid - vapour, solid - liquid, solid - vapour, equilibria) and also gives a short account of three-component systems, including systems of three liquids, ternary eutectic systems and aqueous salt solutions. There is also a useful chapter on experimental methods related to most of the types of system treated in the earlier pages. This book may also be recommended to those chemists who may be “out of practice” with the phase rule and are looking for a quick revision course. S. J. GREGGMarch, 19671 BOOK REVIEWS 203 INTRODUCTION TO ELECTRON SPIN RESONANCE. By H. M. ASSENHEIM. Pp.viii + 200. London: This book is the first in a set of Hilger monographs on electron spin resonance and, as its title implies, it is an introduction to the subject. The second to be issued is reviewed below and forthcoming titles refer to special classes of materials and to instrumentation. These samples and the authorship of the future volumes suggest that the venture will be a useful one. This particular work covers the entire subject and the balance of the different aspects seems just right. It is written from a fundamentally practical approach, but the theory is not neglected. Those seriously interested in the subject for the first time, including undergraduates, should find this account valuable. The style is generally clear and helpful, and a single rapid reading should leave a bird’s eye impression of the field.This book is fairly reliable, although there are a few unfortunate errors. The subject is one that tends to lie between physics and chemistry, and readers trained in either discipline should profit equally. The research specialist will not find much that is novel or of great interest and must wait for the later, more advanced, volumes. Readers of The Amlyst will be aware that electron spin resonance is not a major tool in the analyst’s locker. It is, however, almost essential on the rare occasion when the problem concerns free radicals in the solid or liquid state. It also has its place if weak concentrations of transition or rare-earth metal ions are significant. There are better ways of detecting such impurities, but in suitable cases electron resonance will identify the metal valency and the geometry of its surround- ing co-ordinated ligands.Analysts who wish to learn more about the technique will find this account a good starting point and will certainly expect to find this book in their libraries. Hilger & Watts Ltd. 1966. Price 42s. D. H. WHIFFEN ELECTRON SPIN RESONANCE IN SEMICOXDUCTORS. By G. LANCASTER. Pp. viii + 152. London: And as might be expected it is a t a more advanced level suitable for research workers entering the field. Besides the specific electron resonance topics it forms a useful introduction with more general aspects of semiconductor theory. The main chapters concern both deep and shallow traps in silicon, germanium and 111-V compounds and also defects introduced by radiation damage.The reviewer is not very knowledgeable in this detailed field and he found the ideas well presented a t the level he would have chosen. There is sufficient mathematics to make a good introduction to research papers and an appendix on the Wannier functions. A general analyst will seldom be called on to examine semiconductors. Those who do meet this problem will be aware that impurities have a major influence on the electrical properties. They should find food for thought in this book and be aware of the ability of electron resonance not merely to identify any paramagnetic impurity but also to give a detailed account of the electron distribution. D. H. WHIFFEN Hilger & Watts Ltd. 1966. Price 42s. This is the second published book in the series referred to in the last review.CHEMICAL STUDY OF SOME INDIAN ARCHAEOLOGICAL ANTIQUITIES. N. S. RAWAT. and New York: Asia Publishing House. 1965. Price 15s. By SATYA PRAKASH and Bombay, Calcutta, New Delhi, Madras, Lucknow, London This monograph, issued under the auspices of the State Council of Scientific and Industrial Research of the Government of the State of Uttar Pradesh, presents the results of analyses carried out by the authors and other investigators on a wide range of Indian archaeological materials. The first two chapters are devoted to the analysis of ancient Indian mortars and plasters (mostly from Mohenjo-daro, Harappa and Kausambi) and ceramic materials, including glazes and pottery pigments. This is followed by a chapter in which the results of the analysis of glass objects excavated from various sites throughout India are discussed, and the last two chapters are con- cerned with the analysis of copper and bronze objects and ancient Indian coins.This monograph is essentially a compilation of analytical results collected from many sources, and, as such, it is a convenient book of reference for the chemist who is interested in archaeology. Its value, however, would have been greatly increased if the authors had given some indication of the actual methods of analysis used, and had offered some critical comments about the methods of analysis and the problem of obtaining representative samples. Information of this kind is necessary if one wants to make valid comparisons of analyses made by different investigators. Pp.iv + 100.204 BOOK REVIEWS [Analyst, Vol. 92 The authors have rightly drawn attention to the fact that often there is a great need for further analytical work to be carried out on a systematic basis, before it will be possible to draw definite conclusions of archaeological significance about the composition of ancient Indian objects of different periods and from different localities. Nevertheless, these analytical results have led to some interesting tentative conclusions about the extensive use of lime plaster throughout ancient India, the development of the glazed-tile industry, and the origin of ancient glass at Taxila. For certain Indian coins, the analytical results have been supplemented by metallographic examination.From these studies it was deduced that silver coins and bronze coins containing a high percentage of tin or lead had a cast structure, whereas copper coins showed evidence of an annealed and worked structure. The monograph is well produced and reasonably free from misprints ; it should, however, be noted that the columns for “grams” and “grains” in Table 6.2 (p. 69) have been reversed. A. E. A. WERNER TECHNIQUES IN FLAME PHOTOMETRIC ANALYSIS. By N. S. POLUEKTOV. Translated by C. NIGEL TURTON and TATIANA I. TURTON. Pp. xvi + 219. Princeton, New Jersey, Toronto, New York and London: D. Van Nostrand Company Inc. Originally published in Russia in 1959, this work is a paperback reprint edition of the English translation that was first printed in the United States of America in 1961.The text falls into two distinct sections in which the first four chapters describe the fundamental principles of flame photometry, apparatus, factors affecting sensitivity and accuracy, and photometric measurements. The second section emphasises the practical aspects of flame photometry, and gives details for the determination of alkali, alkaline-earth metals, boron, aluminium, iron and manganese, etc., as applied to a wide range of materials. The book concludes with a useful appendix, in which wavelengths of the strongest spectral lines of various elements are given, and here an indication of the relative sensitivities would have been useful. There have been several important developments in flame photometry since this book was first published, e.g., the use of instruments that incorporate automatic background correction, and many elements are now determined with increased sensitivity after a preliminary extraction of the metal complex into an organic solvent, followed by direct aspiration of the extract into the flame. The bibliography is extensive, and although most of the references are a t least 10 years old, this is inevitable in a double publication such as this.The table of contents is reasonably detailed, but the addition of an index would have been useful. Over-all, this volume gives a useful account of flame photometry, and should provide a basis for an understanding of the subject, bearing in mind its original date of publication. 1966. Price 40s. H. PUGH THE ANALYSIS OF NICKEL.By C. L. LEWIS, W. L. OTT and N. M. SINE. Pp. x + 214. Oxford, 1966. Although the literature contains many papers dealing with the determination of individual impurities in nickel, the only previous comprehensive compilations of modern methods are to be found in the American and British standards for the analysis of the grades of nickel used in the electronics industry. This new book is the first monograph that endeavours to provide a complete guide for the analyst concerned with nickel containing less than 1 per cent. of alloying constituents. The authors have not attempted an encyclopaedic coverage but have mainly limited them- selves to those methods which they have tested and adopted for use within their own organisation. Of necessity this has meant some bias towards the requirements of the produccrs of nickel; the needs of specialist users have not always been covered.Apart from this minor criticism, this book can be highly recommended. No volumetric or gravimetric procedure is advocated by the authors; in accordance with the best modern practice, preference is given wherever possible for optical and X-ray spectrochemical methods of wide applicability. These are supported by a range of spectrophotometric methods and limited applications of polarography, flame photometry and atomic-absorption spectrophoto- metry. Separate chapters deal with sampling, the determination of carbon and sulphur, and the determination of gases. London, Edinburgh, New York, Toronto, Paris and Braunschweig : Pergamon Press. Price 55s.March, 19671 BOOK REVIEWS 205 The expert metallurgical analyst will appreciate the authors’ mastery of their subject and will find a useful collection of well tried and well presented methods.The young journeyman analyst should obtain rather more from reading this book, for it demonstrates admirably how the competent industrial analyst chooses from the many available techniques to obtain the desired results as cheaply, rapidly and efficiently as possible. C. H. R. GENTRY BIOCHEMICAL PREPARATIONS. Volume 11. Edited by ANDREAS C. MAEHLY. Pp. xii + 147. New Volume 11 follows the pattern of former volumes in the now indispensable series of Biochemical Preparations, but each year the variety of substances described seems, if that were possible, to grow more varied and intriguing. In this volume the preparations described range from com- paratively simple chemicals such as acetyl-P-methyl choline and 2-acetamido-2-deoxy-a-D-glucose (better known as N-acetyl-glucosamine), both made by chemical synthesis, to a crystalline protein (ceruloplasmin) prepared from blood plasma and complex molecules such as mesoporphyrin IX, ribonucleic acid and diguanosine tetraphosphate also prepared from natural sources or, as with thymidine polynucleotides, by synthesis.Of particular value to the biochemist are the descriptions of methods for isolating and purifying the enzymes, cytochrome oxidase, enolase, gluconate phosphate dehydrogenase and lactate dehydrogenase. Twenty-five preparations are given in all. The practice adopted in developing the methods described is the same as with previous volumes, in that a method submitted by the original research worker is checked independently by another worker.In most instances footnotes are appended giving the checker’s comments where he wishes to elucidate a point, suggest an improvement or call attention to some difference between his results and those of the original workers. As is customary, instructions are given in such detail that no one should have difficulty in operating the procedures described. The subject index is of particular value as it lists all the preparations described in the preceding ten volumes as well as the current one. Another useful feature is an index of compounds of biochemical interest which have appeared in the forty-five volumes of Organic Syntheses. The book is well bound in strong blue covers that should stand up to the rough handling a laboratory manual may be expected to receive.York, London and Sydney: John Wiley & Sons Inc., 1966. Price 60s. F. A. ROBINSON THE RADIOCHEMICAL MANUAL. Edited by B. J. WILSON. Second Edition. Pp. 137. Amersham: The second edition of The Radiochemical Manual incorporates both parts of the original publication, but has been revised, enlarged and re-arranged so that many of the earlier criticisms no longer apply, although it must still be used in conjunction with the Radiochemical Centre Catalogue. The aim of this manual “. . . is to help the individual user-the scientist, doctor, engineer, or technologist-to choose the right (radioactive) material for his particular purpose and to make effective use of it,” and this aim is largely fulfilled by the provision of extensive information on the properties of radioactive materials and detailed discussion of the problems concerned in their use.The first half of the manual consists of a well written text covering the general nature of radioisotopes, the production process, the synthesis of labelled compounds and the manufacture of radiation sources (chapter 1 to 4) ; various problems involved in the production, use and measure- ment of radiochemicals (chapter 5 to 10) ; details of radiological safety, waste disposal, transport and legislation concerning the use of radioactive substances (chapters 11 to 13) ; and a compre- hensive reading list of journals, abstract journals, books and other publications that cover the subject (chapter 14).Each chapter includes extensive and up-to-date references, but these can be difficult to locate and would have been more convenient if in the form of footnotes or if grouped together in a single bibliography. There has been an obvious attempt to rationalise the style of the different chapters, but with so many contributors there still remains a certain amount of duplication and a lack of uniformity, particularly in the use of commas. Typographical errors are, however, very few for a publication of this size. The second half of the book comprises some fifty tables which cover physical data for the commoner isotopes (it is difficult to see why certain short-lived isotopes are included when some longer-lived ones are omitted), characteristics of radiation sources, synthesis and decomposition of labelled compounds, measurement techniques and safety.A 17-page index, which is both extensive and accurate, completes an extremely useful manual that is well produced and represents good value for the intending user. The Radiochemical Centre. 1966. Price 50s. D. GIBBONS206 BOOK REVIEWS [Analyst, Vol. 92 SPOT TESTS IN ORGANIC ANALYSIS. By FRITZ FEIGL, ENG., D.Sc., and DR. VINZENZ ANGER. Translated by RALPH E. OESPER, PH.D. Seventh English Edition. Pp. xxiv + 772. Amsterdam, London and New York: Elsevier Publishing Company. 1966. Price 170s. This new edition of Feigl’s “Spot Tests in Organic Analysis” makes a welcome appearance six years after the publication of the sixth edition.In the preparation of this new text, Professor Feigl has enlisted the help of Dr. Anger, a colleague and protagonist of spot-test analysis ; the result is a completely revised, re-organised and enlarged text, Room for the considerable amount of new material has been found in two ways; by an increase in the number of pages from 675 to 772, and by deletion of the general chapter on spot-test techniques (which is identical with the chapter in the author’s “Spot Tests in Inorganic Analysis”). Inessential tables and structural formulae have been severely pruned from the earlier text. The total number of tests is now over 900-an increase of about 300 on the previous edition. An important feature of the new edition is the inclusion of two entirely new chapters, one dealing with tests for the detection of particular structures and certain types of organic compounds, and the other with the differentiation of isomers and homologous compounds, and the determination of constitution .Despite the enormous growth of physical methods for the identification of organic compounds, direct chemical methods still have a wide application and, of course, are simpler, easier and very reliable. Surprisingly, these chemical methods can sometimes succeed where the most sophisticated instrumentation fails. This serves to emphasise the premier position of this volume in the literature of qualitative organic analysis. Quite apart from its great utility as a manual of spot tests which can be applied in the most diverse ways, this book is an invaluable source for reaction chemistry, albeit exploited for purely qualitative analytical purposes.The printing and binding are of the usual high standard with which Elsevier are invariably associated, and form an admirable complement to the excellence of the text. The author’s personal researches and inspiration to his many colleagues have led, within the space of twenty years, to the development and consolidation of this highly significant branch of analytical chemistry. No laboratory con- cerned with either pure or applied organic chemistry in any of the diverse fields can afford t o be without this new volume. This is, without doubt, the finest edition yet of Feigl’s “Spot Tests.’’ WILLIAM I. STEPHEN THE INVESTIGATION OF ORGANIC REACTIONS. By Ross STEWART. Pp. xvi + 125. London, Sydney, Toronto, Delhi and Tokyo : Prentice-Hall Inc. 1966. Price (cloth) 44s. ; (paper) 20s. In this book the broad outlines of physical organic chemistry are presented in a form suitable for students about to embark on a degree course. If the remaining nine volumes in the Foundations of Modern Organic Chemistry Series are as clearly written, the enterprising teacher and the eager student will have a feast of good things a t their disposal. Professor Ross Stewart is a prominent investigator in the field of reaction mechanisms, which doubtless accounts for the clarity of ex- pression and the refreshingly novel outlook that persists throughout the book. In Chapter 1, starting from elementary thermodynamical concepts the various factors affecting equilibria in organic systems are described. Chapter 2 deals with reaction intermediates and their electronic structures, and is followed by a brief section on the transition states of organic molecules (Chapter 3). In Chapter 4, which discusses reaction paths, the concepts developed in the previous chapters receive more extended treatment. In this section a good balance is struck between the functional and reaction mechanism aspects of organic chemistry. The final chapter deals with catalytic phenomena, illustrated with reference to such diverse phenomena as condensation reactions, Friedel - Craft syntheses, free radical polymerisation, enzyme reactions and so on. Besides suggestions for further reading, a t the end of each chapter several thoughtful problems are given, for whose solution many students will need the guidance of an experienced tutor. A good index is provided and the price of the paper-backed edition is not unduly high for such a valuable monograph. F. G. ANGELL

ISSN:0003-2654    

DOI:10.1039/AN9679200201

出版商:RSC    

年代:1967

数据来源: RSC

摘要:

206 BOOK REVIEWS [Analyst, Vol. 92 Erratum JANUARY (1967) ISSUE, p. 65, correction to p. 30 of “Official, Standardised and Recommended Fov “Dilute standayd coppev solutiolz, ’’ vead “Stvong standavd coppev Methods of Analysis.” solution.”

ISSN:0003-2654    

DOI:10.1039/AN9679200206

出版商:RSC    

年代:1967

数据来源: RSC