Characterisation of Viscosity and Molecular Weight of Fractionated NR
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1 Characterisation of Viscosity and Molecular Weight of Fractionated NR ENG A.H. Science & Technology Innovation Centre, Ansell Shah Alam, Malaysia ( Abstract Viscosity of a rubber solution depends on concentration, temperature, type of solvent, and molecular weight of the rubber. For a particular solvent, the intrinsic viscosity, [η], measured at a specific temperature is related to its molecular weight, M, by the equation [η]=km a, where K and a are Mark-Houwink constants. In this study, fractionated natural rubbers were obtained by adding methanol to toluene rubber solution, while the viscosity by viscometry. The molecular weight of the rubbers was determined by membrane osmometry and 13 C-NMR techniques. The [η] values of the rubbers were found to increase from 1.1 to 8.0 as the molecular weight increased from 7x10 5 to 1.1x10 7 g/mol. The Huggin s constant, k, which is known to be independent of molecular weight or molecular weight distribution but usually increases with the degree of branching, was observed to increase from 0.4 to 0.8 with increasing molecular weight of the rubbers. This indicates the presence of higher degree of branching in the higher molecular weight fractions. The branching was estimated from molecular weight data and found to increase from 1 branching point per chain for the low molecular weight faction to 5 branching points per chain for the high molecular weight fraction. The plot of log [η] versus log (M) produced a linear regression. The linear regression was found to be significant at 95% confidence level (P=0.001). From the intercept of the plot, K = 2.99 x 10-4 dl g -1 was obtained by calculation, while the gradient corresponds a = INTRODUCTION The molecular weight distribution of natural rubber obtained from Hevea brasiliensis has a broad molecular weight distribution. Depending on the clonal origin, these molecular weight distributions can be categorized 1 into 3 types as described in Table 1 1. Table 1: Different types of molecular weight distribution of natural rubber 1 Type Description 1 Distinctively bimodal distribution with the low molecular weight and high molecular weight regions having about the same peak height. 2 Distinctively bimodal distribution with the low molecular weight region s peak height half or less than half of that of the high molecular weight region 3 Skewed unimodal distribution with a flat slope in the low molecular weight region.
2 The molecular weight, M, can be correlated to the viscosity of the rubber solution by the Mark-Houwink equation, as shown in Equation 1. [η]=km a, where K and a are the Mark-Houwink constants 1 Equation Due to the wide molecular weight distribution, the constants for natural rubber are normally obtained by fractionating the rubber and determining [η] and M values of each fraction with narrow molecular weight distribution. Several K and a values for natural rubber determined in different solvents and at different temperatures have been reported 2. However, some of these have no experimental details, i.e. from unpublished results. Therefore, the experiments were carried out in this study to confirm the K and a values in these reports. EXPERIMENTAL Field natural rubber latex was obtained from regularly tapped rubber tree of RRM600 clonal origin. It was stabilised with 0.7% ammonia after collection. 1% w/v of sodium dodecyl sulphate (SDS) was added to the latex before being deproteinized using 0.02% w/v Alcalase 2.0T enzyme (Nova Nordisk) after 2 days of latex collection. The reaction conditions were conducted at 37 o C for 16 hours at ph 9.5. Upon completion, the latex was centrifuged at 11,000-13,000rpm (17,000 20,000g) for 30min. The cream fraction was re-dispersed in 1% and the centrifugation repeated. The cream fraction was then isolated and the rubber coagulated by methanol, washed extensively with water and dried under reduced pressure at room temperature to constant weight. The nitrogen content was 0.01%w/w as determined by the Kjeldahl method. Fractionation of the natural rubber was carried out by stepwise addition of methanol to 1% w/v stirred toluene solution at 30 o C. Upon the formation of precipitate, the methanol addition was stopped, and the temperature of the stirred solution was slowly raised to between o C until the precipitate dissolved. The heating and stirring were then discontinued, and the solution was allowed stand and cool slowly to 30.0 o C overnight. The precipitated rubber was isolated and the fractionation on the toluene solution continued until all the rubbers had been isolated. Such fractionation method produced natural rubber of narrow molecular weight distribution. Viscosity of the rubber in toluene solution was measured with an Ubbelohde viscometer at 30.0 o C. The intrinsic viscosity was then determined from the Huggins equation as shown in Equation 2. η sp /c = [η] + κ [η] 2 c Equation 2 where c is the concentration of the rubber solution in g/dl -1, [η] intrinsic viscosity, and κ Huggins constant. No corrections were made for the shear rate dependence intrinsic viscosity. Molecular weight of the rubbers was determined by a Wescan 231 Membrane Osmometer. Regenerated cellulose membrane designated as RC 51
3 for use in non-aqueous medium, was supplied by Schleicher & Schuell, Germany. The membrane was allowed to equilibrate in toluene for 7 days after several gradual conditioning steps, before installing it into the osmometer cell. The osmotic pressure of 4 to 5 rubber toluene solutions in the range of 1.5 to 5g dm -3 were measured in the order of increasing concentration. Triplicate analysis was carried out on each rubber solution and the average results were reported. Each osmotic pressure, π was then divided by the associated concentration, c and this value, π/c, was plotted against the rubber concentration, c. A best fit regression was plotted and extrapolated to zero concentration. The intercept, (π/c) c=0 was used for the number average molecular weight determination according to Equation 3. M n = RT/ (π/c) c=0 Equation 3 where R and T are gas constant and absolute temperature, respectively. The accuracy of the instrument was verified by the use of three standard polystyrene samples and found to be within a deviation of 5%. 13 C-NMR measurements were carried out on deuterated chloroform solution of rubbers with tetramethylsilane (TMS) as internal standard using JEOL FX-200 spectrometer under the conditions shown in Table 2. Table 2: Conditions for 13 C-NMR measurement Sample concentration 10% w/v Temperature 50 o C Observed frequency 50.1 MHz Sweep width 10,000 Hz Point 16,000 Pulse width 10 µs Pulse interval 12 sec Scan 30,000-40,000 RESULTS AND DISCUSSION Five fractions of natural rubber were fractionated. However, only the first four fractions were used and the last fraction was excluded in this study because it normally contains a high level of impurities. The intrinsic viscosity, the corresponding Huggins constant, κ, and the molecular weight for each fraction of the rubber are given in Table 3. Branching* Table 3: Intrinsic viscosity and molecular weight of fractionated natural rubbers Fraction Intrinsic Huggins Molecular weight, M n x viscosity, constant, 10-5 [η] κ Osmometry 13 C-NMR*
4 *Based on peak intensity ratio of cis/trans isoprene **Branching = M n (Osmometry)/M n (NMR) 1 It is well known that for a given polymer, the Huggins constant, κ, is independent of molecular weight and molecular weight distribution. However, it is increased by a decrease in solvent power. Most significantly, κ is increased by the incidence of branching in the polymer chains 3. For linear polymers in thermodynamically good solvents, values of about 0.3 are usually observed. In the case of linear synthetic cis polyisoprene, much lower values of 0.2 are normally found 3. The κ values for the fractionated rubbers shown in Table 3 are much higher than 0.2, indicating the presence of branching, the level of which increases with increasing molecular weight. The presence of long chain branching in soluble fractions of natural rubber is very probable since the branching can eventually lead to the formation of insoluble gel, which is a crossslinked entity normally present in natural rubber, leading to the phenomenon of storage hardening. In an earlier study 4, it was also found that the extent of storage hardening increased with increasing molecular weight. This confirms that higher molecular weight fractions have a stronger tendency to form branching and crosslinking reactions, as shown in Table 4. Table 4: Plasticity of various fractions of natural rubber Fraction Intrinsic viscosity Extent Initial plasticity, P o Accelerated storage hardened plasticity*, P H of hardening, P= P H - P o *At 60 o C for 24 hours with phosphorous pentoxide as a desiccant From the 1 H-NMR studies 5, it has been demonstrated that each rubber chain contains 2 trans isoprene units. Assuming that these trans isoprene units remain intact after the branching reaction, each high molecular weight molecule is then consisting of several linear molecules each having 2 trans isoprene units. On the basis of this assumption, the branching point in each rubber fraction was determined from the ratio of M n, measured by osmometry to that by 13 C-NMR as shown in Table 3. The degree of branching for the fractionated rubbers agrees well with that of the values of Huggins constant, κ, i.e. increases with increasing molecular weight. This confirms the findings reported by two other groups of researcher using a different technique 6,7. A comparison was made among the three results as shown in Figure 1. The results of present study were found to be closer to the tri-functional branching point model of Angulo-Sanchez and Caballero-Mata 6.
5 Based on the Mark-Houwink equation shown in Equation 1, a plot of log [η] versus log M n is expected to give a linear correlation. Figure 2 shows that such linear regression is obtained in the present study. The correlation was found to be statistically significant at 95% confidence level (P<0.001). The gradient of 0.74 corresponds to the a value in the Equation 1. From the value at the intercept, K = 2.99x10-4 dl g -1 was obtained by calculation. These values are comparable to the unpublished results of Subramaniam 1, where he quoted the values of a=0.71 and K=3.31x10-4 dl g -1 in his paper in However, there were no experimental details given in the paper. A further literature search in Polymer Handbook revealed that there were no Mark-Houwink constants published on natural rubber in toluene at 30 o C. A further comparison can be made with synthetic cis polyisoprene 8, which was measured in toluene solution at 30 o C, as summarized in Table 5. Table 5: Mark-Houwink constants for natural rubber and synthetic cis polyisoprene in toluene at 30 o C. Sample K x 10 4 a Reference Synthetic cis polyisoprene Natural rubber , 9 Natural rubber Present study REFERENCE 1. SUBRAMANIAM, A. (1972) Gel Permeation Chromatography of Natural Rubber. Rubb. Chem. Technol., 45, SUBRAMANIAM, A. (1980) Molecular Weight and Molecular Weight Distribution of Natural Rubber. Rubb. Res. Inst. Malaysia Technol. Bull. No BRISTOW, G.M. (1962) The Huggin s κ Parameter for Polyisoprenes. J. Polym. Sci., 62, S168-S ENG, A.H. (1989) Storage Hardening of Natural Rubber. M. Sc. Thesis, University of Malaya, Malaysia. 5. ENG, A.H., KAWAHARA, S., AND TANAKA, Y. (1994) Trans-Isoprene Units in Natural Rubber. Rubb. Chem. Technol., 67, ANGULO-SANCHEZ, J.L. AND CABALLERO-MATA, P. (1981) Long Chain Branching in Natural Hevea Rubber Determination by Gel Permeation Chromatography. Rubb. Chem. Technol., 54, FULLER K.N.G. AND FULTON, W.S. (1990) The Influence of Molecular Weight Distribution and Branching on Relaxation Behaviour of Uncrosslinked Natural Rubber. Polymer, 31, KURATA, M. AND TSUNASHIMA, Y. (1989) Viscosity-Molecular Weight Relationship and Unperturbed Dimension of Linear Chain Molecules, Polymer Handbook, BRANDRUP, J. AND IMMERGUT, E.H. ed., pp. VII/1- VII/60, John Wiley & Sons. 9. SUBRAMANIAM, A. (1993) Characterisation of Natural Rubber. Proc. Int. Rubb. Technol. Conf. Kuala Lumpur, pp
6 (Reference 6) (Reference 7) (Reference 6) Figure 1: Branching points and molecular weight of natural rubber
7 y = x Log [η] Log [MW] Figure 2: Relationship between molecular weight and intrinsic viscosity of NR
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