Detailed Investigation of Modulus of Elasticity in Linseed Oil-impregnated Mature Norway Spruce Sapwood Thomas Ulvcrona 1 ABSTRACT Various techniques and preservatives are used in wood preservation, some of which are toxic. Hence, there is a need for further development (and use) of non-toxic alternatives, such as linseed oil impregnation by the Linotech process, especially for wood such as mature sapwood from Norway spruce (Picea abies L. Karst.) with anatomical features that make it difficult to impregnate with preservatives by currently applied industrial processes. In the study reported here we examined the modulus of elasticity (MOE) of sub-samples of mature Norway spruce sapwood impregnated by this process to evaluate its effects, caused by possible structural damage, on the wood’s short-term mechanical properties. Two sets of process settings were applied, “low” and “high” with treatment times, pressures and temperatures of 2 and 3 h, 0.8 and 1.4 MPa, 60 and 140˚C, respectively. The treatments resulted in 30-50% mass increases in the specimens. MOE was generally slightly lower in control (unimpregnated) specimens than in specimens impregnated at low and high settings (9976, 10663 and 10528 MPa, respectively). The results indicate that the Linotech process does not cause more structural damage than drying without impregnation, and that determination of short-term mechanical properties followed by basic statistical analysis provides a convenient means for detailed evaluations of effects of varying process settings. KEYWORDS Short-term mechanical properties, Hydrophobic oil, Method development. 1 Swedish University of Agricultural Sciences Unit for Field-based Research Svartberget Fieldstation SE-922 91,Vindeln SWEDEN, [email protected] Thomas Ulvcrona 1 INTRODUCTION Right now there is worldwide a constant evaluation of possible sustainable processes that could substitute many of the environmentally adverse preservation techniques currently used. As one of many potential processes, impregnation of wood with hydrophobic oils has already been extensively evaluated for many years. Potential sustainable alternatives to many currently used environmentally adverse preservation techniques are being intensively sought. One of many potential processes, impregnation of wood with hydrophobic oils, has been known for many years, but further evaluation and development of the process is still required. Previous studies have shown that it is possible to successfully impregnate even recalcitrant types of wood, such as mature sapwood from Norway spruce (Picea abies L. Karst), with the linseed oil product Linogard® using the Linotech process [Ulvcrona et al. 2006, Ulvcrona & Bergsten 2007]. In this process the linseed oil does not enter the cell wall structure, but the moisture uptake of the resulting wood-based material is retarded by the formation of a hydrophobic layer within the wood [Fredriksson et al. in press]. Thus, it probably does not affect the chemical (and hence structural) contents of the cell walls. However, the temperatures that may be used in the process are relatively high (60-140 °C) and external pressure may also be applied [Ulvcrona et al. 2006, Ulvcrona & Bergsten 2007], so it could potentially cause structural changes resulting in alterations of short-term mechanical properties. Accordingly, Wang [2007] has reported that impregnation with oils can have structural effects that might restrict use of impregnated materials in constructions. Thus, clarifying the effects of hydrophobic oil impregnation on wood’s short-term strength properties is an important first step towards elucidating the potential range of uses for wood treated with hydrophobic oil. Thus, in the presented study the Modulus of Elasticity (MOE) of mature Norway spruce sapwood impregnated by the Linotech process with two sets of process settings was investigated. 2 MATERIALS AND METHODS 2.1 Samples In total, 15 Norway spruce (Picea abies L. Karst) trees from three stands in a mixed coniferous forest in northern Sweden (64°10’N, 160-320 m above sea level) were selected, from each of which in all more than 60 samples (500*25*25 mm) were sawn from the mature sapwood. A third of the samples (controls) were dried, but not impregnated, a third were impregnated by the Linotech process with “low” settings (2 h treatment at 0. 8 MPa and 60-140˚C) and the other third by the process with “high” settings (3 h treatment at 1.4 MPa and 140˚C). The moisture content of the wood (percentage of wood dry mass) before impregnation was calculated according to standard method EN 384 [1995]. The impregnation resulted in 30-50% increases in the mass of the mature sapwood specimens, and their linseed oil contents were calculated as a percentage of wood dry mass. For further details of these procedures, see Ulvcrona et al. [2006]. 2.2 Modulus of Elasticity and Macroscopic Cracks Forty impregnated mature sapwood samples were randomly chosen to test their MOE, as a general indicator of their mechanical properties, and eight unimpregnated mature sapwood samples were randomly chosen as controls. The top half of each sample was cut longitudinally with a band saw to form nine specimens of equal size (219*6*6 mm) with standing annual rings according to Fig. 1, then specimens representing each treatment, and control specimens, were randomly selected for the MOE measurements according to Table 1. In addition, material properties of the samples (moisture content and density) prior to impregnation, and their oil contents post-impregnation, were determined to assess possible correlations between these variables and the specimen’s MOE values. 2 XII DBMC, Porto, PORTUGAL, 2011 Modulus of Elasticity in Linseed Oil-impregnated Mature Norway Spruce Sapwood Figure 1. Sketch showing the sawing pattern of specimens from the samples. Tests were performed using an Instron Universal, 10 kN testing machine with standard equipment for 3-P bending. All specimens were loaded until failure, using a crosshead speed of 4 mm minute-1. Displacement of the crosshead was recorded and used to calculate the strain. Thus, the absolute flexural modulus values are not entirely correct, but are still useful for comparisons between reference and impregnated specimens. Specimens were conditioned and tested at 23°C with 50% humidity. The elastic flexural strain, ε , on the bottom surface was calculated as: fl (1) εfl = 6w0h/l 2 where w0 is the measured deflection, and h is the thickness of the specimen. Flexural stress, σfl, was calculated as: 2 (2) σfl = 3Pl / 2h b where P is the applied load, and b is the width. The flexural modulus, E , was calculated, in MPa, as: fl (3) Efl = σfl / εfl with measurements of applied load taken between 0.01 – 0.05 kN chosen for calculations. The shear factor was neglected in the calculations of flexural modulus because the l/h ratio (26.7) made it insignificant [Kollman & Cote, 1984]. The bending strength, ƒm, was calculated, in MPa, as: (4) ƒm = aFmax / 2W according to standard method EN 408 [1995]. Macroscopic crack development was measured with the naked eye and a caliper across the whole (25*25mm2) surface in the middle of samples before further sawing into specimens. 2.3 Statistical Analysis All statistical calculations were performed using MINITAB software [Anon., 1999]. The data were tested for normality and heteroscedasticity, and the results indicated that no transformations were needed. To test for differences in mean values related to the treatments One-way Anova was used. XII DBMC, Porto, PORTUGAL, 2011 3 Thomas Ulvcrona 3 RESULTS AND DISCUSSION There were no easily interpretable general trends concerning effects of process settings on the Modulus of Elasticity (MOE) values of the mature Norway spruce sapwood specimens impregnated by the Linotech process [Table 1], although they were slightly lower for untreated specimens than for impregnated specimens [Table 1]. However, MOE values of untreated specimens were not significantly lower than those of specimens impregnated with high settings [Table 1]. The standard deviation of the MOE values was also slightly lower for the unimpregnated specimens [Table 1]. Table 1. Mean (and standard deviation), minimum and maximum Modulus of Elasticity (MOE) values of samples following the applied treatments (numbers of investigated specimens in brackets). Treatment Mean (MPa) MOE Standard Deviation Untreated Low settings 9976a (48) 10663b (107) Variance 1330 1556 1556 1568 MOE Minimum (MPa) 6643 5593 MOE Maximum (MPa) 13666 14255 High settings 10528ab (95) 1568 1330 7983 14480 Note, superscript letters indicate significant differences between treatments according to Tukey’s tests at the 0.05 probability level. This tallies to some degree with findings reported by Megnis et al. [2002], who also discuss the possibility that hydraulic effects of oil present in the cavities may increase the wood’s stiffness in compression , which in turn affects its MOE and strength. However, the levels of uptake in the investigated samples seem to have been insufficient to significantly alter the short-term mechanical properties of the impregnated wood. There appears to have been no more structural damage after impregnation than after drying without further treatment. Among the examined specimens, there were no significant differences between impregnation treatments regarding linseed oil uptake; the mean values of oil uptake were 25.4% of wood dry mass for both impregnation treatments (not further presented). No significant differences in macroscopic crack development were found either following the investigated impregnation treatments; mean values of macroscopic crack development were 6.6 and 5.8 mm, in treatments with “low” and “high” settings respectively (not further presented). Scatterplot of MOE 2 vs Density; MOE 3 vs Density 2 300 MOE 2*Density 15000 325 350 375 400 MOE 3*Density 2 12500 10000 7500 5000 300 330 360 390 420 Figure 2. MOE of specimens impregnated by the Linotech process with “low” (MOE 2) and “high” (MOE 3) Linotech settings in relation to the samples’ wood density (kg/ m3) before impregnation. 4 XII DBMC, Porto, PORTUGAL, 2011 Modulus of Elasticity in Linseed Oil-impregnated Mature Norway Spruce Sapwood There were also no significant differences between treatments regarding wood density before impregnation in the investigated samples [Fig. 2]. Wood density is generally quite strongly correlated with MOE in samples with otherwise similar variables. There were weak indications of this correlation in the specimens subjected to the Linotech process with “low” settings, but no such indications in the specimens subjected to the process with “high” settings [Fig. 2]. There were also no significant differences between treatments regarding wood moisture content before impregnation in the investigated samples [Fig. 3]. Scatterplot of MOE 2 vs mst ct bef; MOE 3 vs mst ct bef2 50 MOE 2*mst ct bef 15000 100 150 MOE 3*mst ct bef2 12500 10000 7500 5000 50 75 100 125 150 Figure 3. MOE of specimens impregnated by the Linotech process with “low” (MOE 2) and “high” (MOE 3) settings in relation to their wood moisture content (%) before impregnation. Previous studies have shown that the wood moisture content (expressed as water-filled porosity) is positively correlated with uptake of oil in the Linotech process [Ulvcrona et al. 2006, Ulvcrona & Bergsten 2007]. However, the moisture content before impregnation of the samples examined here did not have any apparent effect on the MOE of the impregnated wood material [Fig. 3]. Scatterplot of MOE 2 vs linseed oil perc; MOE 3 vs Linseed oil perc 10 MOE 2*linseed oil percentage 15000 20 30 40 MOE 3*Linseed oil percentage 2 12500 10000 7500 5000 0 10 20 30 40 Figure 4. MOE of specimens impregnated by the Linotech process with “low” (MOE 2) and “high” (MOE 3) settings in relation to the samples’ linseed oil percentage (%). XII DBMC, Porto, PORTUGAL, 2011 5 Thomas Ulvcrona In addition, there were no significant differences between treatments regarding uptake of oil, expressed as linseed oil percentage of wood dry mass before impregnation in the investigated samples [Fig. 4]. Wang [2007] has reported that impregnation with oils can cause structural changes in impregnated materials that might restrict their use in constructions. However, we found no clear trends regarding effects of linseed oil uptake on the MOE of the resulting wood material [Fig. 4]. It should be noted the levels of oil uptake were generally similar following impregnation by the process with both sets of settings [Fig. 4]. Therefore, it is difficult to draw conclusions regarding possible effects of all levels of oil uptake. However, this study provides information about effects of impregnation to levels likely to be applied in commercial practice. This study shows that the presented methodology can be used to study, in detail, the effects of variations in process settings on the short-term mechanical properties of impregnated wood, providing a convenient approach for optimizing parts of the process in screening studies before progressing to large-scale studies of short-term mechanical properties in full-scale products. Further, use of highly characterized raw wood materials allowed much of the natural variability present in wood from whole trees to be excluded, providing opportunities to highlight effects of separate parts of the process. In addition, the study indicates that impregnation with linseed oil in the Linotech-process does not have major effects on the MOE of mature Norway spruce sapwood. Possible hydraulic effects in the wood are not significant when samples are divided into specimens. Neither do any of the investigated material properties have any obvious effect on MOE in the investigated samples. Finally, the absence of clear negative effects of the investigated impregnation process on MOE indicates that further investigations of its effects on both the short-term and long-term mechanical properties of full-scale products are warranted. However, such investigations should be done in parallel with studies like this, allowing effects of specific process settings to be identified. ACKNOWLEDGEMENTS The author thanks The Swedish University of Agricultural Sciences theme research program “Future Forests” for financial support and Sees-Editing for professional editing. REFERENCES Anon. EN 384. 1995. Structural timber – determination of characteristic values of mechanical properties and density, European standard 384. European Committee for Standardization. 1-8. Anon. EN 408. 1995. Timber structures – Structural timber and glued laminated timber – Determination of some physical and mechanical properties, European standard 408. European Committee for Standardization, 1-19. Anon. 1999. Minitab Statistical Software Release 13 for Windows. Fredriksson, M. Ulvcrona, T. & Wadsö, L. 2010. ´Swelling and moisture sorption of Norway spruce (Picea abies L. Karst.) impregnated with linseed oil´, Wood Material Science and Engineering. In press. Megnis M., Olsson T. Varna J. & Lindberg H. 2002. `Mechanical performance of linseed oil impregnated pine as correlated to the take-up level`, Wood Science and Technology, 36[1], 1-18. 6 XII DBMC, Porto, PORTUGAL, 2011 Modulus of Elasticity in Linseed Oil-impregnated Mature Norway Spruce Sapwood Kollman, F.F.P. & Cote, W.A. 1984. Principles of Wood Science and Technology, Vol. 1 Solid Wood, Springer Verlag, Berlin. Ulvcrona, T. Lindberg, H. & Bergsten, U. 2006. ´Impregnation of Norway spruce (Picea abies L. Karst) wood by hydrophobic oil and dispersion patterns in different tissues`, Forestry, 79[1], 123-134. Ulvcrona, T. & Bergsten, U. 2006. `Possibilities for compositional tailoring of Norway spruce (Picea abies L. Karst.) wood using a hydrophobic oil impregnation process`, Holz als Roh- und Werkstoff, 65[2], 167-169. Wang, J. 2007. Initiating evaluation of thermal-oil treatment for post-MPB lodgepole pine, Forintek Canada Corp., Vancouver BC, Canada. XII DBMC, Porto, PORTUGAL, 2011 7
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