Characterization of A New Fiber from Cyperus Dichrostachus A . Rich Plant

Natural fibers are of the good substitute sources for swaing synthetic fibers and reinforcing polymer matrices because of their contributions in maintaining of ecology, low energy requirement for processing and sustainability. The aim of this study is to characterize new fiber from Cyperus Dichrostachus A. Rich (CDA) plant. The CDA plant is a perennial non woody grass found in Ethiopian high lands and river basins. The fiber from this plant has chemical composition of Cellulose (60.27%), hemicellulose (22.72%), lignin (16.59%) contents. It has a density of 1010 kg/m 3 and good tenacity behaviour of 105.76 cN/Tex with low elongation of 4.88%. The thermal stability of Cyperus Dicrostachys A . Rich fiber (CDAF) was studied using TGA and DTG analysis and revealed that the cellulose degraded at a temperature of 377.1°C. Fourier transform-infrared spectroscopy analysis confirmed that CDAF is rich in cellulose content. Additionally, CDAF can play a vital role as new reinforcement material and best alternative in bio composite industries. This will give competitive advantages when evaluated with other natural fibers reveals that there are significant potential benefits in implementation of cleaner production in textile material production industries. Specifically, replacement of synthetic fiber source with renewable biomass will reduce the environmental impact of these fibers. The future study will entail on investigating the possible valorization route especially in paper board, composite reinforcement and bio composite alications. cellulose The with and with and for though magnetic the flask an additional portion of 2.0 g sodium chlorite and ml acetate and the continued again for an hour. After at room for 45 a dispersion of holocellulose out into 500 mL beaker and settled overnight. The sediment of holocellulose was washed with hot and finally with distilled up to a neutral separating the liquid phase from holocellulose by sedimentation overnight. The washed holocellulose was in the Aluminium sheet at 105 ° to constant weight. Then the percentage of holocellulose the extracted CDAF


INTRODUCTION
It has been obvious that numerous natural plants have been grown in different provinces of the world with fluctuating atmospheric conditions, grown in agricultural domains and after their lifetime, end up in landfills [1,2] , e-ISSN: 2321-6212 method was used for further evaluation of the effect of extraction methods that ranks the means and calculates the minimum value to be significantly different with each other at p ≤ 0.05. From the ANOVA tables, fit summary, signalto-noise ratio value, Predicted R² value and diagnostic plots, the significance of the models were checked and finally, the optimized factors were determined and rework of extraction at the optimized extraction technique was done.
Characterization methods: In order to determine the suitability of using extracted CDA fiber as a renewable fiber source for the production of high-value materials, it was important to understand their physical and chemical properties. In this section methods of such comprehensive characterization are reported.
Physical properties: The characterizing of physical properties of the fiber was characterized well after the extraction process as described by the following sections.
Fiber density: The density of the CDA fiber was measured using a liquid pycnometer and the chemicals used were distilled water, paraffin and acetone. Five replicates were performed for each sample type and the density was calculated using equation (1) Where ρt=is the density of distilled water (g/cm 3 ), m1=is the mass of empty pycnometer (g), m2=the mass ofpycnometer with fibers (g), m3=the mass of pycnometer with distilled water (g) and m4=the mass of pycnometer with fibers and distilled water (g) [44] .

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Optical microscopic analysis: The aspect ratio, shape of the fiber, and diameter of the fiber were measured using optical microscope. For fiber diameter analysis, thirty five distinct fiber samples have been considered; and from the microscopic images were taken along the longitudinal direction [45] . The diameter was measured by the microscope built with video analyzer and camera. After calculating the average value of diameter, the diameter of extracted CDAF was compared with various plant fibers.
Linear density: The count of the extracted fibre was calculated in Tex units and measured by single-fiber weighing method through which the length of a single fiber was measured and the fiber was weighed as per the ASTM D 2257 standard. Then linear density (Tex) was estimated using equation (2) to compare the fineness of the extracted fiber with other plant fibers.
Diameter: The diameter of CDA fibers obtained from the single cells was studied using an optical Microscope, built in video analyser LEIKA to measure the thicknesses of the single fibers as per the ASTM D3171 (1990) standard.
Statistical analysis was done to compare the fiber diameter between CDAF and other fibers [45].  (4) Where; W=Weight of water in the fibers (g); O=oven dry fiber weight (g) Thermal property analysis: A thermo-gravimetric Analyzer, TGA 4000 Perkin Elmer machine was used to measure the degradation characteristics, the mass and transformation of CDAFs in nitrogen atmosphere with flow rate of 20 ml/min [44,46,47] . All the measurements were examined with aluminum crucible [48] for good coupling between the e-ISSN: 2321-6212 sample and the temperature measured by the thermocouple in a temperature range from 30°-700°C at a heating rate of 20℃/min.
Analysis of chemical composition: Chemical analysis was performed to determine the contents of cellulose, hemicellulose lignin, wax, moisture, and ash of CDAFs by following conventional chemical analysis techniques as stated in Figure 2 [49,50] . Chemical analysis of the extracted CDAF was performed by adapting TAI methods [51,52] . Estimation of lignin content: The TAI T222 method [53] was used with pre-hydrolysis of the extracted sample with 72 wt. % sulfuric acid at room temperature for 2 hrs to determine the content of acid-insoluble lignin [51,54,55] . Then the concentrated acid was diluted with distilled water, and the sample was hydrolyzed with dilute 3% acid at boiling temperature for 4 hrs. Thereafter, the acidic dispersion of lignin was filtered through filter paper having average pore size of 11 μm. The residue of lignin was washed on the filter with hot water up to neutral pH followed by drying at 105°C to constant weight. Accordingly the extracted CDAF sample 3 g was mixed with 150 mL of 72 % sulfuric acid in 500-ml flask and pre-hydrolyzed at room temperature for 2 hrs [55] . The concentrated acid was diluted with 3450 mL distilled water and the sample was hydrolyzed with dilute acid on a heating plate at boiling temperature for 4 hours using flask beakers. After cooling at room temperature for 30 min, the acidic dispersion of lignin settle overnight and the liquid phase becomes transparent.
The sediment of lignin was washed with hot water and with distilled water to a neutral media, separating the liquid phase from lignin by sedimentation followed by filtration with a filter paper. The washed lignin was dried with aluminum sheet at 105°C to constant weight. The percentage of acid-insoluble lignin [56] in the extracted fiber sample was calculated by the equation [54,57] : P -Pt AIL = 100% Ps [57] Where P is weight of dry acid-insoluble lignin with Aluminum sheet; Pt. is weight of empty aluminum sheet; and Ps is weight of extracted and dried CDAF sample.

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Estimation of cellulose and hemicellulose content: The determination of cellulose and hemicellulose was based on the separation of holocellulose which contain both cellulose and hemicelluloses. First the extracted CDAF sample, 2 g, was placed into 200 ml flask, and then160 mL distilled water, 2.0 g sodium chlorite (NaClO2) and 4 mL glacial acetic acid were added into the flask. The flask was covered with Petri dish and put into a water bath with a temperature of 90°C and treated for 1 hr though magnetic stirring. Then to the flask an additional portion of 2.0 g sodium chlorite and 4 ml acetate buffer was added, and the treatment was continued again for an hour. After cooling at room temperature for 45 min, a dispersion of holocellulose was poured out into 500 mL beaker and settled overnight. The sediment of holocellulose was washed with hot water, and finally with distilled water up to a neutral pH, separating the liquid phase from holocellulose by sedimentation overnight. The washed holocellulose was dried in the Aluminium sheet at 105°C to constant weight. Then the percentage of holocellulose in the extracted CDAF was calculated by equation 6 [57] : Where P is weight of dry holocellulose together with aluminium sheet; Pt. is weight of empty aluminium sheet; and Ps is weight of extracted and dried CDAF sample [53,54] . Then the content of cellulose was achieved from holocellulose hydrolyzed with dilute hydrochloric acid to remove hemicelluloses based on the TAI T201 wd-76 and The dried holocellulose sample was mixed with 180 mL of 2% HCl in 500-ml flask, and the sample was hydrolyzed with the dilute acid at boiling temperature for 2 h followed by cooling at room temperature for 30 min. then the acidic dispersion of cellulose was segmented overnight for 1 hr. The sediment of cellulose was washed with hot water, and finally with distilled water to a neutral pH, monitored by separating the liquid phase from cellulose by sedimentation and filtration with a filter paper. Then the cellulose was dried in aluminum sheet at 105°C to constant weight. The percentage of cellulose and hemicelluloses in the extracted CDAF was calculated as Cellulose(C) and Hemicellulose (H) in the extracted CDAF respectively in equation (7 and 8):   HC * p -Pt C= Ps (7) and Where HC is percentage of holocellulose; P is weight of dry cellulose together with flask; Pt. is weight of empty flask; and Ps is weight of extracted and dried biomass sample.
Fourier Transform Infra-Red (FTIR) spectroscopy: FTIR Spectrometer, Spectrum (Perkin Elmer) was employed to identify the functional groups present in the CDA fibre [46,58] . The sample was compressed using a mechanical pressure pellet maker for 1 minute at 65 kg/cm 2 pressure condition to form pellets of small sizes. The spectrum was recorded in the range of 4000 to 400 cm -1 with 32 scans per minute and with the resolution of 4 cm -1 .
Longitudinal analysis of the fiber: The longitudinal interface of the fibre under a Microscope, built in video analyser LEIKA [58] showed that the fibre has some convolutions and twisted structures along its length with smooth, uniform and good aearance as illustrated in Figure 4. The convolutions outfit for comfortable and comparable characteristics of the fiber as in cotton. Moisture regain: The moisture regain of CDAF was 12.40 ± 1.75% and the moisture content was 11.01 ± 1.38%.
CDA fiber has a good and comparable moisture property like other natural fibres. The comparison of the physicalproperties and tensile properties of CDAF with other few natural fibers is presented in Table 2. Thermo gravimetric analysis: It is obvious that natural fibers encompass cellulose, hemicellulose, and lignin, by which their amount contributes for the thermal stability of the fibers. Consequently, the degradation temperatures of these components of CDA fiber play a noteworthy role to assess the thermal stability of its constituents. Moreover, the thermal stability of the CDA fiber components was studied to estimate the oortunity of its alication as reinforcement in composite and other manufacturing sectors. The Thermo Gravimetric Analysis (TGA) and Derivative Thermo Gravimetrics (DTG) of CDA fiber is shown in Figure 5. The initial degradation of the fiber is noticed (at e-ISSN: 2321-6212 82.2°C) between room temperature and 109°C; this was due to the dehydration of the fiber [64] . The succeeding foremost degradation evolved from the temperature region of 110-410.5°C in which a peak quite close to 167.6°C related to thermal depolymerisation of hemicelluloses, and some fraction of cellulose and lignin components [65] with 22.9% of mass loss. Hemicellulose started its decomposition easily, with the weight loss mainly haened at 220-330℃ [65] . A precise noticeable peak at 377.1°C revealed a major mass loss of about 66.3% due to the breakage of glycoside bonds of cellulose and alpha and beta alkyl ether linkages of lignin (Kommula et al., 2016) lead to the degradation of cellulose. Similar results were also observed at 331.1°C for Prosopis juliflora, 321°C for bamboo, 308.2°C for hemp, 298.2°C for jute and 309.2°C for Kenaf fibers [63] . Figure 5 show that there is little difference only in % mass loss rate of the CDA fiber. This shows that part of the foreign matter and organic components have been removed by the alkali treatment and increase the percent loss and contribute for some amount of mass loss rate in the fiber. reaction of the fiber [66] . From the analysis of the DTG curve of CDA fiber, it has shown that after moisture removal from the sample, the primary decay peak was in the temperature range of 268. °C) that corresponds to the thermal destruction of cellulose components [67] .
The second peak was positioned within the range of 410.5-607.5°C with the maximum at 486.9°C that follows the maximum rate of lignin thermal destruction [68,69] . Therefore, from the DTG curve it can be justified that the fiber has more amount of cellulose than hemi-cellulose and lignin components. The summary is shown in Table 3. Dehydration of moisture present in the fiber (11.2 %) [70] 110°-410°C Thermal depolymerisation Hemicelluloses, and some fraction of cellulose and lignin components [65] 220-330℃ Decomposition Loss (22.9%) of Hemicellulose [65,71] 377.1°C Breakage of glycoside bonds of cellulose α and β aryl-alkyl-ether linkages of lignin Degradation (57.1%) of cellulose [70,72] Analysis of chemical composition The chemical composition of CDAF is presented in Table 4. CDAF has estimated cellulose content of 60.27 ± 9.3% which is higher than that of kenaf (53.  The above Figure 6 shows that there is a significant difference in chemical composition of the CDA plant before extraction and the chemical composition of the extracted fiber. This shows that part of the lignin and hemicellulose components have been removed by the alkali treatment and increase the number of OH groups and contribute for the high amount of cellulose in the fiber. As shown in Table 4; CDAF contains optimum hemicellulose (22.72 ± 0.32%) and high lignin (16.59 ± 0.32%) contents. The optimum hemicellulose content has given good contribution for biodegradation, moisture absorption, and thermal decay of the fibre [73] . Higher ranges of lignin help to retain water within the fiber, which safeguards the fiber from biological attacks [61] .
Furthermore CDA fiber has 1.55 ± 0.003% extractives of wax and pectic substances which comprises less portion of wax content that enhance easier composite production for the fact that the bond between the matrix and the fiber become higher for fabricating of the composite structures with this fiber. When compared with other natural fibers just like Flax (1.5-1%), Sisal (2%), Nettle (3.1-4.2%), Okra (3.9%) and Abaca fibers (3%) have comparably higher percentages of wax content than CDAF which has 1.55% of wax. The lesser percentage of wax enables chemical treatment, and it can also afford an improved cohesive bonding between the fiber and composite matrix [55] .
The ash content (1.3%) of CDAF was found to be lower when compared to other natural fibers like Cyperus pangorei (3.56%), Prosopis juliflora (5.2%). The data showed that lighter composites can be prepared by using CDAF in polymer matrices. CDA fiber has similar properties in composition with Cyperus pangorei fibers of 68.5% cellulose, 17.88% lignin, 0.17% wax, 9.19% moisture content and 1102 kg/m 3 density [64] .
More importantly the chemical composition of the CDAF has compared with different plant fibers as shown in Table   5 and revealed that the fiber has comparable chemical composition in all aspects.
e-ISSN: 2321-6212 Table 5. Comparison of chemical composition of CDAF [45,60,74,75] . FTIR analysis: Fourier-transform infrared spectroscopy is utilized for characterizing lingo cellulosic fiber to identify chemical compounds in a wide range of capacities, by considering the infrared features and transmittance bands of their constituents [76] . The FT-IR spectrum of CDA fiber is presented in Figure 7 and the detailed is shown in Table 6.
The spectral graphs create the functional group sketch of the fiber, a distinguishing molecular fingerprint that can screen out and scan samples for diverse components of the fiber, and detect functional groups, distinguish the covalent bond relationship figures. In general, from the FTIR result of CDAF, we can conclude that the fibre has very well-known chemical compounds the can be depicted from their functional groups. Its composition of the functional groups is comparable with other well-known natural cellulosic fibres.

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Stretching of C-O due to the vibration of the acetyl group Lignin [81] 1164 C-O-C groups asymmetric bridge stretching, Hemicellulose and cellulose molecules [81] 1055 C-O aromatic ring and skeletal vibration of C-O-C Cellulose [81] 895 βglycosidic linkages between the sugar units Hemicellulose and cellulose molecules [82] 690 C-H bond of aromatic hydrogen Lignin compound [82] 523 Out of plane bonding of OH [82] e-ISSN: 2321-6212

CONCLUSION
We Now days, the need for recyclable, renewable and sustainable materials has brought about the amplified consumption of natural fibers for reinforcing polymers to outfit a wide variety of alications. This study was mainly focused on the extraction and characterization of the lignocellulosic fiber derived from Cyperus Dichrostachus A.
Rich plant. On the progress of this study, the new natural lignocellulosic fiber was successfully demonstrated to be an alternative source for producing fiber for varied alications. The fiber was extracted warm water extraction techniques at different NaOH concentrations. The influence of alkali treatment with correlated factors and extraction techniques on the chemical composition, morphological, structural, thermal and tensile properties of the fiber was studied well.
The elimination of hemicellulose from the fiber strands on this fiber was proved by chemical analysis and FT-IR studies. The thermal stability of the fiber strands was found to be better-quality for warm water extracted fiber treated with NaOH.