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Sadhan Basu – a Physical Chemist Extraordinaire a Glimpse Into His Research Work

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Sadhan Basu – a Physical Chemist Extraordinaire a Glimpse Into His Research Work GENERAL ARTICLE Sadhan Basu – A Physical Chemist Extraordinaire A Glimpse into his Research Work Ramprasad Misra and S P Bhattacharyya Sadhan Basu was an inspiring teacher and sci- entist and among the best that our university system has produced. He carried out impor- tant and thoughtful research work in the ¯elds of polymers, spectroscopy and quantum chemistry (left) Ramprasad Misra did that bear the signature of a highly creative mind. his doctoral studies And all these he did with so little resources at (integrated PhD) in S P his disposal. No wonder that his memory still Bhattacharyya’s research group at IACS and is inspires awe and respect among many of his im- presently in the mensely successful students and colleagues. University of Pittsburgh. His research interests are in Sadhan Basu (1922{1992) was a physical chemist in the physical organic true sense of the term. Possessed with a fever of cre- chemistry and molecular ative thinking, he pursued research with rare zeal in spectroscopy. practically all areas of physical chemistry { polymers, (right) S P Bhattacharyya, kinetics, spectroscopy and theoretical chemistry. He at- Fellow of the Indian tracted the best students and his group in the University Academy of Sciences, retired College of Science and Technology in Kolkata (then Cal- as Senior Professor of cutta) became very famous. He was a dedicated teacher physical chemistry, IACS, and enjoyed teaching. He was indeed an illustration of Kolkata in March 2012 and is presently at IIT Bombay how teaching and research could wonderfully comple- as Raja Ramanna Fellow ment each other in a university set up. After a brief (DAE). His main research stint in the Lac Research Institute, Ranchi, Basu started interest is in the area of his research career in Physical Chemistry in India in the quantum chemistry. year 1948 when he joined the Indian Association for the Cultivation of Science (IACS), Kolkata { the cradle of Indian science, established in 1876. A few years later, he moved to take up a teaching position in the Uni- versity of Calcutta (C.U.). Much later, he became the Keywords Chain transfer kinetics, charge Director of IACS, a job he did not perhaps relish. He transfer complexes, mechano- went back to C.U. as Palit Professor, after a brief stint chemical effect, phthalocya- in IACS as the Director. He never went for big budget nines. projects and shunned publicity. The research he carried 598 RESONANCE July 2013 GENERAL ARTICLE out, however, had the unmistakable stamp of brilliance that dazzled all and inspired many. In what follows, we shall focus on Basu's work in the early years of his ca- reer in India which began with a foray into the realm of physical chemistry of polymers (1950). Polymerization Kinetics The prevailing ideas at that time were based on kinetic data on bulk polymerization and it was assumed that the degree of polymerization was equal to the kinetic chain length. That is, the stabilization of the growing polymer molecule and destruction of its activity for growth took place simultaneously. Kinetic data on polymerization in solution that were then just coming in, however indicated that the rate of polymerization in solution was virtually the same as that in the bulk while the degree of polymerization predicted from solution data was invariably lower than its bulk polymerization counterpart. Moreover the plots of log P against log A (where P and A are the degree of polymer- ization and monomer concentration, respectively) were not linear as would have been expected. The best lin- ear ¯t produced straight lines with slopes less than one (< 1). One was therefore forced to conclude that the growth of the polymer chain in solution was being ter- minated by a process that did not stop polymerization. P J Flory1 (1937) hypothesized that the growing poly- 1 See Resonance, Vol.8, No.6, mer molecule could transfer the activity for growth to a 2003. solvent molecule, a monomer molecule or another poly- mer molecule. Initial work by Suers et al (1937), Schultz (1938{39), Mayo (1943) on polymerization of styrene in solution led to evaluation of chain transfer e±ciency of Basu pioneered the a few solvents. study of kinetics of Basu et al (1950) in two landmark papers [1{2] critically catalyzed and examined Flory's hypothesis through a large number uncatalyzed chain of carefully planned experiments on both uncatalyzed transfer and catalyzed chain transfer polymerization kinetics of polymerization. RESONANCE July 2013 599 GENERAL ARTICLE methyl methacrylate in more than 25 solvents. The highlights of the study were (Box 1): 1. Evaluation of chain transfer e±ciency of a large number of solvents and relating the e±ciency to structural features of the molecules. Box 1. Kinetics of Chain Transfer Polymerization in Solution, Catalyzed or Uncat- alyzed 1. A generalized derivation given by Basu et al [1] proceeds as follows: Let A, B and M1¤ be the monomer, catalyst and the activated molecule, respectively. The bimolecular initiation reaction, then reads K1 A + B M¤ : (i) ¡! 1 The propagation step consists of successive addition of the monomer (A) to M1¤. K2 K2 K2 M ¤ + A M ¤ + A M¤ + A : : : M ¤ : (ii) 1 ¡! 2 ¡! 3 ¡! n The deactivation/stabilization then involves K3 Mn¤ + Mm¤ or (2Mn¤) Mm+1 + Mm 1 or M2n : (iii) ¡! ¡ The growing molecule could transfer its activity to a monomer (A) or solvent molecules leading to Ktr M ¤ + A M + A¤ (iv) n ¡! n Ktr M ¤ + S 0 M + S¤ (v) n ¡! n KS S¤ N¤ ; ¡! where S stands for solvent molecules and N ¤ the active radical formed by the interaction between an active solvent molecule and the monomer. The number average degree of polymerization (P¹) is simply the ratio of the velocity of chain propagation and velocity of chain termination; so, ¹ K1[A][C¤] P = 2 ; (vi) K3[C¤] + Ktr[A][C¤] + Ktr0 [C¤][S] Box 1. Continued... 600 RESONANCE July 2013 GENERAL ARTICLE Box 1. Continued... where [C¤] denotes the overall concentration of the active free radical. When the rate at which active centres are produced becomes equal to the rate of their destruction, we have 2 K1[A][B] = K3[C¤] (vii) whence, 1 2 K1 [C¤] = [A][B] (viii) K ½ 3 ¾ Using [C¤] given by equation A8 in equation A6, we have 1 1 K1K3[B] 2 Ktr = f g 1 + (ix) P¹ (K + K )[A] 2 K2 + Ktr 2 tr µ ¶ ¸[S] = ; (x) [A] Ktr # where ¸ = 0 is called the chain transfer constant . [K2+Ktr] Ktr Since, Ktr K2, one writes ¸ = 0 ¿ K2 2. In bulk polymerization [S] and Ktr0 are equal to zero, whereby 1 1 K1K3[B] 2 Ktr = f g 1 + (xi) P¹0 (K + K )[A] 2 K2 + Ktr 2 tr µ ¶ 3. For uncatalyzed bulk polymerization B = A so that for this case we have 1 1 K K 2 K = f 1 3g + tr (xii) P¹ (K + K ) K + K 0 2 tr µ 2 tr ¶ The corresponding equation for uncatalyzed polymerization in solution then reduces to 1 K [S] 1 1 ¸ [S] 1 = tr0 + or; = £ + (xiii) P¹ K + K [A] P¹ P¹ [A] P¹ ½ 2 tr ¾ 0 0 4. The crucial question regarding the bimolecularity/unimolecularity of the initiation 1 [B] step was answered by examining the features of plots of P¹ against [A] and the ex- q1 [B] perimental data obtained by Basu et al (II) showed that the plots of P¹ against [A] were linear with slope independent of [A], which con¯rmed bimolecular initiation.qThe 1 p[B] features of plots of P¹ against [A] rejected the idea of unimolecular initiation. # 1 [S] [B] ¸ was determined from the slopes of plots of P¹ against [A] at constant [A] . Box 1. Continued... RESONANCE July 2013 601 GENERAL ARTICLE Box 1. Continued... The monomolecular initiation leads to 1 [B] [S] K = K + ¸ + tr P¹ [A] [A] K p 2 1 p[B] and predicts that the plots of P¹ against [A] should be linear at all monomer concen- 1 [B] trations while the plot of P¹ against [M] would reveal changing slope with change in monomer concentration which was noqt the case experimentally. 2. Demonstration that the kinetic model of chain trans- fer was equally applicable to catalyzed and uncat- alyzed polymerization in solution. 3. The initiation step was unambiguously identi¯ed to be bimolecular. Basu continued his research in polymer chemistry for a while. His ability to innovate was striking. End- group titration was then a popular and useful method for the determination of molecular weights of polymers. Basu [3] noted that because of the insolubility of certain 2 2 Nylons are condensation co- nylons in common organic solvents, it was not possi- polymers formed by dicarboxy- ble to apply the end-group titration technique to all ny- lic acids and diamines, the most lons. Taking cue from S R Palits's observation that weak common variant being nylon 6-6 bases could be conveniently titrated in organic solvent, obtained from hexane dioic acid and hexane 1,6 diamine. with a solution of perchloric acid in glycolic mixtures, he went on to dissolve nylon in phenol containing a small amount of glycol and titrated it electrochemically with dilute perchloric acid (0.01 N { 0.1 N) in 1:1 glycol{ isopropyl alcohol mixture. Assuming that there was one free primary amino group at the end of each polymer chain, and noting the locations of the in°exion points in the observed pH versus volume of acid-added plots, the molecular weight could be correctly estimated. Swelling{Deswelling of Polymers The ingenuity of Sadhan Basu and his ability to de- sign simple experiments to demonstrate the working of 602 RESONANCE July 2013 GENERAL ARTICLE a physicochemical principle is amply illustrated by his design of the mechanochemical Carnot engine.
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