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Gel permeation chromatography
BOOK REVIEWS the use of disc electrophoresis that the pulmonary surfactant mixture does not contain any serum type lipoprotein, whereas M. Galdston and D. O. Shah present evidence that lipoproteins are present. A. Rothen and C. Mathot report a study of immunological reactions carried out at the interface between monolayers transferred to metalized glass slides and solutions. I. J. Moore presents certain analogies between sugar transport across human erythrocyte membranes and the translocation of sugars from aqueous to a butanol phase. P. W. Brandt and K. B. Hendel report on the permeability of amoeba plasma membrane to polar nonelectrolytes. The above papers, as well as those not mentioned here constitute an interesting collection for all those who wish to learn more about advances at the interface between physical chemistry and biological studies. HENRI L. ROSANG
Department of Chemistry City College of New York New York, New York Gel P e r m e a t i o n Chromatography. Edited by KLAUS H. ALTGELTAND LEON SEGAL. Dekker, New York, 1971. 646 pp. $24.75. Since the introduction of gel permeation chromatography (GPC) by J. C. Moore, of the Dew Chemicals Company in the early sixties as a means of fractionating high polymers, it has been generally recognized as the most important technique in polymer characterization. In the past 8 years, a tremendous amount of experimental and theoretical work has emanated to serve the needs arising from different areas of application. Involved scientists have been anticipating the appearance of a book which exhaustively summarizes the past efforts and critically reviews the advances in this field. This book was published at the right time and fulfills such a purpose. It is a well-edited compilation of the proceedings of the American Chemical Society Symposium on GPC, February 22-27, 1970 in Houston, which first appeared in 19701971 issues of Separation Science. The beginning section of the book provides a review of basic background material to enable the novice to follow later papers of a more advanced nature. Also, it serves as a guide in applying the principles to a specific application. With this idea, the book is divided into four parts: I. Fundamental Introduction to GPC; II. Reviews of Theory and Evaluation Methods in GPC; III. New Developments in GPC; and IV. Applications of GPC to Problems in Polymer and Petroleum Chemistry. The first paper in part I illustrates the basic separation mechanism which adopts molecular size as its discriminant. The pictorial representation of the compatibility between statistical
675
size of polymer coils and internal pore dimensions of the column packing is most instructive. The next two papers describe the functionality, desirable properties, and available types of both column packings and detectors for effluent analysis. In the fourth paper, the concept of GPC resolution is presented. Elegant reviews of the mathematical models of the various contributions to peak broadening from mobile phase and stationary phase; and reviews of the methods for correcting symmetrical and unsymmetrical peak spreading are given in the last three papers of part I. In part II, the first paper provides concrete experimental evidences in supporting the view that lateral diffusions in the mobile phase and the stationary phase are the primary sources of peak dispersion. Also, given verification are Herman's theory of permeation dispersion and Casassa's model of equilibrium partitioning. One may find it helpful to grasp the qualitative outlook and general terminology (such as viscous fingering), from this paper and the first paper of part I I I before reading the paper by Kelley and Billmeyer in part I, which reviews various peak dispersion models. The second paper in part I I by E. F. Cassassa introduces a thermodynamic model, which describes the equilibrium distribution of unperturbed random flight chains in the mobile phase and the accessible void space in the cavity of the column packing. Such mathematical formulation of permeation should prove to be interesting reading material to polymer chemists. Of the last two papers in part II, the former presents the concept of hydrodynamic volume of solute molecules as the universal calibration variable for column calibration; and the latter describes the process of data interpretation and corrections. Parts I and II essentially constitute a good introductory textbook to GPC, in which the separation concept, description of packing materials and instrumentation, calibration of column set, mathematical models of peak dispersion and permeation mechanism, and data interpretation are all included. For actual practice in correcting peak dispersion and column calibration, the following papers are highly recommended as supplements to the discussions in parts I and II: (i) The two papers in part I I I by Provder and Rosen on instrumental spreading correction with linear and nonlinear calibration curves. Their approach is an elegant extension of Balke and Hamileac's work [J. Appl. Polym. Sci. 13:1381 (1969)]. (ii) The paper of Provder, Woodbrey, and Clark in part IV. They proposed a general method for obtaining both the molecular weight and hydrodynamic volume calibration curves for polymersolvent systems where primary fractions are not available. With this method, peak dispersion Journal of Colloid and Interface Science, Vol. 38, No. 3, M a r c h 1972
676
BOOK R E V I E W S
cannot be corrected; therefore, experimental conditions must be designed to minimize instrumental spreading. P a r t I I I covers many areas of new development as follows: Methods of characterizing column packing, utilization of recycling to improve resolution, preparative fraetionation, high speed and high load GPC, the effect of temperature and flow rate on peak broadening and resolution; also included are phase distribution chromatography, gel filtration chromatography and the studies of molecular association by GPC. The powerful capability of GPC fraetionation at mild operating conditions is often used in conjunction with other analytical techniques such as differential refractometry, UV, IR, vapor phase osmometry, membrane osmometry, light scattering, N M R , viscometry, density measurements. P a r t IV is a compilation of various combinations of different techniques with GPC for different areas of application. These include the analysis of copolymer composition, degree of polymer branching, plasticizer content, crude oil,
Journal of Colloid and Interface Science, Vol. 38, No. 3, March 1972
petroleum fractions, cellulose fractions, pulps, and pore structure of cotton. As a consequence, a compilation of papers authored by different contributors often unavoidably results in sequence discontinuity. I n t e r m i t tently treated subjects on peak dispersion and column calibration are the most obvious examples. Although as appearing in this book, reviews written by different outstanding researchers who are authorities in the particular fields, are usually most accurate and comprehensive. Generally, the book is easily readable and exhibits more extensive coverage than other similar compilations from previous GPC symposia. I t is highly recommended to newcomers for use as an introductory textbook and to the experienced as an excellent reference book for reviewing the past efforts and recent progress, or as a source for projecting future theory refinement, machine improvement, or new applications. RICHARD K. S. CttAN A i r Products and Chemicals Inc. Allentown, Pennsylvania 18105
Department of Chemistry City College of New York New York, New York Gel P e r m e a t i o n Chromatography. Edited by KLAUS H. ALTGELTAND LEON SEGAL. Dekker, New York, 1971. 646 pp. $24.75. Since the introduction of gel permeation chromatography (GPC) by J. C. Moore, of the Dew Chemicals Company in the early sixties as a means of fractionating high polymers, it has been generally recognized as the most important technique in polymer characterization. In the past 8 years, a tremendous amount of experimental and theoretical work has emanated to serve the needs arising from different areas of application. Involved scientists have been anticipating the appearance of a book which exhaustively summarizes the past efforts and critically reviews the advances in this field. This book was published at the right time and fulfills such a purpose. It is a well-edited compilation of the proceedings of the American Chemical Society Symposium on GPC, February 22-27, 1970 in Houston, which first appeared in 19701971 issues of Separation Science. The beginning section of the book provides a review of basic background material to enable the novice to follow later papers of a more advanced nature. Also, it serves as a guide in applying the principles to a specific application. With this idea, the book is divided into four parts: I. Fundamental Introduction to GPC; II. Reviews of Theory and Evaluation Methods in GPC; III. New Developments in GPC; and IV. Applications of GPC to Problems in Polymer and Petroleum Chemistry. The first paper in part I illustrates the basic separation mechanism which adopts molecular size as its discriminant. The pictorial representation of the compatibility between statistical
675
size of polymer coils and internal pore dimensions of the column packing is most instructive. The next two papers describe the functionality, desirable properties, and available types of both column packings and detectors for effluent analysis. In the fourth paper, the concept of GPC resolution is presented. Elegant reviews of the mathematical models of the various contributions to peak broadening from mobile phase and stationary phase; and reviews of the methods for correcting symmetrical and unsymmetrical peak spreading are given in the last three papers of part I. In part II, the first paper provides concrete experimental evidences in supporting the view that lateral diffusions in the mobile phase and the stationary phase are the primary sources of peak dispersion. Also, given verification are Herman's theory of permeation dispersion and Casassa's model of equilibrium partitioning. One may find it helpful to grasp the qualitative outlook and general terminology (such as viscous fingering), from this paper and the first paper of part I I I before reading the paper by Kelley and Billmeyer in part I, which reviews various peak dispersion models. The second paper in part I I by E. F. Cassassa introduces a thermodynamic model, which describes the equilibrium distribution of unperturbed random flight chains in the mobile phase and the accessible void space in the cavity of the column packing. Such mathematical formulation of permeation should prove to be interesting reading material to polymer chemists. Of the last two papers in part II, the former presents the concept of hydrodynamic volume of solute molecules as the universal calibration variable for column calibration; and the latter describes the process of data interpretation and corrections. Parts I and II essentially constitute a good introductory textbook to GPC, in which the separation concept, description of packing materials and instrumentation, calibration of column set, mathematical models of peak dispersion and permeation mechanism, and data interpretation are all included. For actual practice in correcting peak dispersion and column calibration, the following papers are highly recommended as supplements to the discussions in parts I and II: (i) The two papers in part I I I by Provder and Rosen on instrumental spreading correction with linear and nonlinear calibration curves. Their approach is an elegant extension of Balke and Hamileac's work [J. Appl. Polym. Sci. 13:1381 (1969)]. (ii) The paper of Provder, Woodbrey, and Clark in part IV. They proposed a general method for obtaining both the molecular weight and hydrodynamic volume calibration curves for polymersolvent systems where primary fractions are not available. With this method, peak dispersion Journal of Colloid and Interface Science, Vol. 38, No. 3, M a r c h 1972
676
BOOK R E V I E W S
cannot be corrected; therefore, experimental conditions must be designed to minimize instrumental spreading. P a r t I I I covers many areas of new development as follows: Methods of characterizing column packing, utilization of recycling to improve resolution, preparative fraetionation, high speed and high load GPC, the effect of temperature and flow rate on peak broadening and resolution; also included are phase distribution chromatography, gel filtration chromatography and the studies of molecular association by GPC. The powerful capability of GPC fraetionation at mild operating conditions is often used in conjunction with other analytical techniques such as differential refractometry, UV, IR, vapor phase osmometry, membrane osmometry, light scattering, N M R , viscometry, density measurements. P a r t IV is a compilation of various combinations of different techniques with GPC for different areas of application. These include the analysis of copolymer composition, degree of polymer branching, plasticizer content, crude oil,
Journal of Colloid and Interface Science, Vol. 38, No. 3, March 1972
petroleum fractions, cellulose fractions, pulps, and pore structure of cotton. As a consequence, a compilation of papers authored by different contributors often unavoidably results in sequence discontinuity. I n t e r m i t tently treated subjects on peak dispersion and column calibration are the most obvious examples. Although as appearing in this book, reviews written by different outstanding researchers who are authorities in the particular fields, are usually most accurate and comprehensive. Generally, the book is easily readable and exhibits more extensive coverage than other similar compilations from previous GPC symposia. I t is highly recommended to newcomers for use as an introductory textbook and to the experienced as an excellent reference book for reviewing the past efforts and recent progress, or as a source for projecting future theory refinement, machine improvement, or new applications. RICHARD K. S. CttAN A i r Products and Chemicals Inc. Allentown, Pennsylvania 18105