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Characterisation and Fractioning of Tectona Grandis Bark in View of Its Industrial Crops and Products 50 (2013) 166–175 Contents lists available at ScienceDirect Industrial Crops and Products journa l homepage: www.elsevier.com/locate/indcrop Characterisation and fractioning of Tectona grandis bark in view of its valorisation as a biorefinery raw-material a a a,b a,∗ a Isabel Baptista , Isabel Miranda , Teresa Quilhó , Jorge Gominho , Helena Pereira a Centro de Estudos Florestais, Instituto Superior de Agronomia, Universidade Técnica de Lisboa, Tapada da Ajuda, 1349-017 Lisboa, Portugal b Centro das Florestas e Produtos Florestais, Instituto de Investigac¸ ão Científica Tropical, Tapada da Ajuda, 1349-017 Lisboa, Portugal a r t a b i s c l e i n f o t r a c t Article history: The anatomy and chemical composition of Tectona grandis bark from mature trees in East Timor Received 6 March 2013 are described as well as the characterisation of fractionation by grinding and granulometric Received in revised form 5 June 2013 separation. Accepted 2 July 2013 Teak bark is composed of secondary phloem, periderm and a narrow rhytidome that included various periderms with phloem tissues between them. The layer of phellem cells in each periderm was thin. Keywords: The phloem showed an orderly stratification with tangential bands of fibres in concentric rings that Tectona grandis alternated with thin bands of axial parenchyma and sieve tube elements. Abundant prismatic calcium Teak bark Anatomy oxalate crystals were present. The bark fractured easily into clean particles. The yield of fines was low and 64.4% of the particles were Chemical composition Fractionation over 2 mm. The mean chemical composition of teak bark was: ash 18.5%, total extractives 10.7%, lignin 20.0% and suberin 1.9%. The polysaccharides, corresponding to approximately 47%, showed a predominance of glucose (60.3% of total neutral monosaccharides) and an important content of xylose (20.0%). The content of rhamnose was also comparatively high (4.9%). The content of soluble phenolics was 1.6%. Ash elemental composition showed the predominance of calcium, representing about 93% of the total inorganics, followed by potassium (4.8%) and magnesium (1.9%). Extractives were present preferentially in the fines, with about 30% more extractives than the coarse fraction. Lignin content and monosaccharide composition were similar in the different bark fractions. A difference between fractions was found in relation to suberin content which was lower in the fines: 0.6% and 3.5% in the fine and medium fractions, respectively. © 2013 Elsevier B.V. All rights reserved. 1. Introduction depend on the particular species’ anatomy and physical character- istics (Miranda et al., 2012a, 2012b). Valorisation of residual biomass is a strategic issue in line with Bark is structurally complex and comprises different tissues: present preoccupations regarding sustainability and overall eco- phloem, periderm and rhytidome (Evert, 2006). The phloem logical footprint of materials and energy. Tree barks are interesting includes a functional non-collapsed phloem in the inner part and resources that have large potential since are available in great a non-functional collapsed phloem to the outside; the periderm amounts, i.e. from forest operations and industrial processing, and includes phellogen, phellem and phelloderm; the rhytidome corre- at the same time, barks present a structural and chemical complex- sponds to all the dead tissues isolated by the last formed periderm, ity that make them well suited to integrate biorefinery platforms. i.e. phloem and periderms. In hardwoods, phloem is made up of Prior to processing, barks usually undergo pre-treatments, different cells: the sieve tube elements and associated parenchyma namely of physical nature, to facilitate the subsequent component cells, the axial parenchyma and radial parenchyma cells, the fibres extraction or material use (Wyman, 1999). For instance, mechan- and sclereids. ical fractioning disrupts the cellular tissues and may be used to Due to their structural complexity, bark sampling, characteri- separate fractions of differing composition although fraction yields sation and processing have difficulties that are not found in wood processing. Knowledge on the bark structure is also essential for an estimation of its potential use (Furuno, 1990). Therefore, bark valorisation, namely if envisaged within a biorefinery platform, ∗ requires a careful examination of composition and processing char- Corresponding author. Tel.: +351 21 365 3378. E-mail address: [email protected] (J. Gominho). acteristics. 0926-6690/$ – see front matter © 2013 Elsevier B.V. All rights reserved. http://dx.doi.org/10.1016/j.indcrop.2013.07.004 I. Baptista et al. / Industrial Crops and Products 50 (2013) 166–175 167 Barks are also chemically complex: they are usually rich in sections were mounted on Kaiser glycerine and after 24 h drying, extractives, including organic solvent and water solubles, and in the lamellas were submerged in xylol for 30 min to remove the polyphenolics, and they also contain a high amount of inorganic adhesive, dehydrated on 96% and 100% alcohol, and mounted on material (Fengel and Wegener, 1984; Pereira et al., 2003). Eukitt. In this study we address the case of teak bark. Teak (Tectona Individual specimens were taken sequentially from the cam- grandis L.) grows naturally in South East Asia and is now one of bium towards the periphery and macerated in a solution of 30% ◦ the most important species for tropical plantation forestry, mostly H2O2 and CH3COOH 1:1 at 60 C for 48 h and stained with astra under intensive short rotation management. Teak is one of the most blue. Light microscopic observations were made using Leica DM LA famous timbers in the world, renowned for its dimensional stabil- and photomicrographs were taken with a Nikon Microphot-FXA. ity, extreme durability and strength. The terminology follows mainly in Trockenbrodt (1990) and Richter Teak bark was considered an important fibre resource (Soni et al. (1996). et al., 1980). The bark is rich in tannins and phenolic compounds Teak bark samples were observed by scanning electronic (Babu et al., 2010) and extracts have shown the presence of sterols, microscopy (SEM). The samples were vacuum dried and gold was anthraquinones, triterpenic, hemi-terpenic and naphthalene com- vapour sprayed making up an approximately 450 A thick coating. pounds (Gaikwad et al., 2011; Khan and Mlungwana, 1999). Teak The surfaces were observed in an electron scanning microscope bark is traditionally valued and used as a sweet, acrid astringent to Hitachi S-2400 at magnifications ranging from 50 to 1000×, and treat various anthropogenic ailments such as diabetes, bronchitis, the images were recorded in digital format. The scanning electron constipation and skin diseases, in line with an ayurvedic function microscope was attached to a Bruker EDX (Energy Dispersive X- (Ghosh, 2006; Khan and Mlungwana, 1999; Chopra et al., 1956). Ray Spectroscopy) detector using an acceleration voltage of 20 kV The pharmacognostic and phytochemical use of teak bark were at magnifications of 50–1000×. The images were recorded in digital related to its anatomical structure (Akhtar et al., 2011; Gaikwad and format. Mohan, 2011). The anatomy of teak bark was studied in relation to particular structural aspects (Inamdar and Gangadhara, 1974; 2.3. Fractioning Ghouse et al., 1977), taxonomy (Gottwald and Parameswaran, 1980) and to differentiate from other closely related species The bark with 12% of moisture was ground in a knife mill (Retsch (Goswami et al., 2010). The seasonal development of phloem in SM 2000) using an output sieve of 10 mm × 10 mm and posteri- different regions was also investigated (Lawton and Lawton, 1971; orly sieved using a vibratory sieving apparatus (Retsch AS 200 Rajput and Rao, 1997, 1998; Rao and Rajput, 1999; Dié et al., 2012). basic) with U.S. standard sieves with the following mesh sizes: The bark of T. grandis trees from East Timor has not been char- 80 (0.180 mm), 60 (0.250 mm), 40 (0.425 mm), 20 (0.850 mm), 15 acterised. In this paper we describe the anatomy and chemical (1.0 mm) and 10 2.0 mm. After sieving, the mass retained on each composition of T. grandis bark from mature trees in East Timor for sieve was weighed and the corresponding seven mass fraction which the wood was already studied (Miranda et al., 2011) aim- yields were determined. ing at a full resource valorisation. We also study the fractionation by grinding and the granulometric separation of teak bark. The 2.4. Bark density fractions with different particle sizes were characterised with the objective to analyse the potential of granulometric separation for Bark basic density (p) was determined using oven-dry weight selective component enrichment within a biorefinery route of bark and green saturated volume determined by the water immersion use. method: mp p = 2. Materials and methods Vp 3 2.1. Samples where mp is sample mass (kg), and Vp is sample volume (m ).The determination was made in 5 barks samples. The bark samples were collected from three teak (T. grandis L.) trees harvested in a pure teak stand with 50–60 years of age located 2.5. Bulk density and inter-granular porosity in the northeast of East Timor. A description of site and stand are presented elsewhere (Miranda et al., 2011; Sousa et al., 2012). The bulk density of the granulated samples (at 12% of mois- The trees were randomly selected from dominant trees with ture) was determined for each sieve fraction using a cylindrical 40 cm DBH diameter class, a straight stem and the absence of appar- container (29.8 mm height × 28.1 mm diameter) as the ratio of the ent defects. The harvested trees had the following dimensions: BH sample mass in the container to the volume of the container. The diameters of 40.5, 37.9 and 43.5 cm and heights of 25.0, 22.7 and determination was made in triplicate.
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