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A handbook of decomposition methods in analytical chemistry
Thermochimica Acta, 43 (1981) 123-124 Elsevier Scientific PubIishing Company, Amsterdam -
123 Printed in Belgium
Book Review A Handbook of Decomposition Methods in Analytical Chemistry, Rudolf Bock (translated and revised by Iain L. Marr), International Textbook Company, London, 1979,444 pp., AZ9.75. This is a book dealing with analytical methods based on decomposition methods. The German edition was published in 1972 and, in the Preface to this English edition, author R. Bock points out that the present English text has been expanded considerably and several sections completely rewritten. He expresses the hope that the tables provided can be used without resort to The references are extensive and the book the original publications. throughout well documented. The materials dealt with range over all types of solid samples, both organic and inorganic. The book, however, is organised in terms of various types of procedure. So after an introduction there are chapters dealing with dissolution without chemical reaction, decomposition based on supply of energy, dissolution and opening out by chemical reaction but without change in oxidation state, oxidising procedures, and decomposition procedures involving reduction. Now this is quite an ambitious synopsis and the present reviewer must report that, although ambitious, the chapters deal adequately with the subject matter and the book can indeed be used as a working handbook. In the introductory chapter, there is a very useful section dealing with container materials and the principles governing their choice. The second chapter, dealing with dissolution without chemical reaction, is surprisingly short in view of the industrial importance which this technique has now assumed in, for example, the field of coal chemistry. The next chapter, dealing with decomposition by the action of heat, by photolysis and radialysis, is also surprisingly short. It also deals with mainly organic materials. This must surely be because the classical gravimetric procedures for analysis of inorganic materials are methods dealing with precipitates after the material has been presented to the opening out procedure and do not constitute the initial procedure whereby the original material is converted into a form (usually soluble) suitable for subsequent analysis. There are remarkably few references to thermal analysis being used to investigate this initial procedure and it is possible that herein lies a further extension of thermal analysis methods which might be very popular. The next two chapters contain much more material. The first, Chapter 4, deals with processes which do not involve a change in the oxidation state. This includes dissolution with the aid of complexing agents or ion exchangers, the use of hydrofluoric, fluoboric and fluorosiliac acids, decompositions with ammonium fluoride and ammonium hydrogen difluoride, dissolution with HCl, HBr, or HI, volatilization by heating with ammonium chloride, bromide or iodide, non-oxidizing dissolution with sulphuric acid, fusions with hydrogen sulphates or pyrosulphates, dissolution with phosphoric acids and the use of the phosphate melts, double decomposition with various
124
acids, fusion with boric acid, boron lxioxide or borates, the use of enzymes, pyrohydrolysis, dissolution using alkali metal hydroxides or carbonates with ammonia, hydrazine and organic bases and fusion with alkali metal hydroxides and carbonates. Again, it is d&appointing that the use of thermal analysis methods finds hardly a mention. One method, the Lawrence Smith decomposition method involving heating silicates with a mixture of calcium carbonate and ammonium chloride, may be cited as an example of a reaction which could yield some interesting results when studied by thermal analysis methods. Chapter 5 deals with oxidizing procedures. This includes the procedure known as dry-ashing-heating a sample in an open dish or crucible in air, commonly employed for the combustion of organic matter. This is reported in detail and reading this section provides a wealth of information which could be a useful starting point for thermal analysis investigations. The final chapter, dealing with procedures involving reduction, is much shorter than the two preceding chapters but, here again, there is a section on reduction procedures involving the use of carbon in inorganic and organic analysis which could provide a source of further studies involving thermogravimetric techniques. There is a splendid appendix (Appendix 3) in this book which presents a compilation of decomposition methods satisfactory for routine purposes together with details such as sample amount, decomposition materials, and source reference. This is a very carefully constructed. book, containing useful information for chemists generally. D. DOLLIMORE (Salford, Gt. Britain)
123 Printed in Belgium
Book Review A Handbook of Decomposition Methods in Analytical Chemistry, Rudolf Bock (translated and revised by Iain L. Marr), International Textbook Company, London, 1979,444 pp., AZ9.75. This is a book dealing with analytical methods based on decomposition methods. The German edition was published in 1972 and, in the Preface to this English edition, author R. Bock points out that the present English text has been expanded considerably and several sections completely rewritten. He expresses the hope that the tables provided can be used without resort to The references are extensive and the book the original publications. throughout well documented. The materials dealt with range over all types of solid samples, both organic and inorganic. The book, however, is organised in terms of various types of procedure. So after an introduction there are chapters dealing with dissolution without chemical reaction, decomposition based on supply of energy, dissolution and opening out by chemical reaction but without change in oxidation state, oxidising procedures, and decomposition procedures involving reduction. Now this is quite an ambitious synopsis and the present reviewer must report that, although ambitious, the chapters deal adequately with the subject matter and the book can indeed be used as a working handbook. In the introductory chapter, there is a very useful section dealing with container materials and the principles governing their choice. The second chapter, dealing with dissolution without chemical reaction, is surprisingly short in view of the industrial importance which this technique has now assumed in, for example, the field of coal chemistry. The next chapter, dealing with decomposition by the action of heat, by photolysis and radialysis, is also surprisingly short. It also deals with mainly organic materials. This must surely be because the classical gravimetric procedures for analysis of inorganic materials are methods dealing with precipitates after the material has been presented to the opening out procedure and do not constitute the initial procedure whereby the original material is converted into a form (usually soluble) suitable for subsequent analysis. There are remarkably few references to thermal analysis being used to investigate this initial procedure and it is possible that herein lies a further extension of thermal analysis methods which might be very popular. The next two chapters contain much more material. The first, Chapter 4, deals with processes which do not involve a change in the oxidation state. This includes dissolution with the aid of complexing agents or ion exchangers, the use of hydrofluoric, fluoboric and fluorosiliac acids, decompositions with ammonium fluoride and ammonium hydrogen difluoride, dissolution with HCl, HBr, or HI, volatilization by heating with ammonium chloride, bromide or iodide, non-oxidizing dissolution with sulphuric acid, fusions with hydrogen sulphates or pyrosulphates, dissolution with phosphoric acids and the use of the phosphate melts, double decomposition with various
124
acids, fusion with boric acid, boron lxioxide or borates, the use of enzymes, pyrohydrolysis, dissolution using alkali metal hydroxides or carbonates with ammonia, hydrazine and organic bases and fusion with alkali metal hydroxides and carbonates. Again, it is d&appointing that the use of thermal analysis methods finds hardly a mention. One method, the Lawrence Smith decomposition method involving heating silicates with a mixture of calcium carbonate and ammonium chloride, may be cited as an example of a reaction which could yield some interesting results when studied by thermal analysis methods. Chapter 5 deals with oxidizing procedures. This includes the procedure known as dry-ashing-heating a sample in an open dish or crucible in air, commonly employed for the combustion of organic matter. This is reported in detail and reading this section provides a wealth of information which could be a useful starting point for thermal analysis investigations. The final chapter, dealing with procedures involving reduction, is much shorter than the two preceding chapters but, here again, there is a section on reduction procedures involving the use of carbon in inorganic and organic analysis which could provide a source of further studies involving thermogravimetric techniques. There is a splendid appendix (Appendix 3) in this book which presents a compilation of decomposition methods satisfactory for routine purposes together with details such as sample amount, decomposition materials, and source reference. This is a very carefully constructed. book, containing useful information for chemists generally. D. DOLLIMORE (Salford, Gt. Britain)