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Isolation of cellulose from salacca midrib fibers by chemical treatments
To cite this article: V Yudha et al 2018 IOP Conf. Ser.: Mater. Sci. Eng. 434 012078
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1234567890โ€˜โ€™โ€œโ€
3rd Annual Applied Science and Engineering Conference (AASEC 2018) IOP Publishing
IOP Conf. Series: Materials Science and Engineering 434 (2018) 012078 doi:10.1088/1757-899X/434/1/012078
Isolation of cellulose from salacca midrib fibers by chemical
treatments
V Yudha1
, H S B Rochardjo1*
, J Jamasri1
, R Widyorini4
, F Yudhanto1,2
and S
Darmanto1,3
1
Department of Mechanical and Industrial Engineering, Universitas Gadjah Mada,
55284 Yogyakarta, Indonesia
2
Department of Mechanical Engineering, Universitas Muhammadiyah Yogyakarta,
55183 Yogyakarta, Indonesia
3
Department of Industrial Engineering, Vocation School, Universitas Diponegoro,
Semarang, Indonesia
4
Department of Forest Product Technology, Universitas Gadjah Mada, 55281
Yogyakarta, Indonesia
*heru-sbr@ugm.ac.id
Abstract. Salacca midrib fibers (SMF) have potential as a new source of cellulosic material.
The method of isolate cellulose from SMF carried out by the different stages of chemical
treatment. First stage is alkalization using sodium hydroxide and then second stage is bleaching
treatment using hydrogen peroxide. The chemical composition analysis of SMF was
determined at different stages of chemical treatments. Physical analysis was carried out by
fourier transform infrared spectroscopy (FTIR) and x-ray diffraction (XRD). Change in surface
morphologies of fibers were characterized by scanning electron microscopy (SEM). Isolation
process of cellulose from SMF by alkali and bleaching treatments successfully increased
content of ฮฑ-cellulose, decreased content of lignin and increased percentage of index
crystallinity of fibers.
1. Introduction
Natural fibers can be grouped based on the source that comes from plants, animals or minerals. The
natural fibers of the cultivated plants have the advantage of obtaining and having a shorter harvest
time. Lignocellulosic fibers, also known as cellulose-based fibers, can be devide into nonwood and
wood or plants fiber. Natural fibers are an alternative reinforcement for composite application due to
the environmental issues [1]. The main content of natural fibers is cellulose, hemicellulose and lignin
[2]. Cellulose is renewable, biodegradable and the most abundant natural polymer. Salacca midrib
fibers (SMF) is one of prospective tropical plants to produce fibers from their bast (figure. 1). SMF
has a diameter of 3 to 3,5 cm with a length of 110 cm. The fibers extracted from the bast of salacca
midrib are generally 4-5 years old The chemical composition of raw SMF contain ฮฑ-cellulose 47.18%,
hemicellulose 31.89%, and lignin 22.27% [3].
2
1234567890โ€˜โ€™โ€œโ€
3rd Annual Applied Science and Engineering Conference (AASEC 2018) IOP Publishing
IOP Conf. Series: Materials Science and Engineering 434 (2018) 012078 doi:10.1088/1757-899X/434/1/012078
Figure 1. Salacca midrib fibers.
The isolation proses to separate the cellulose from the extractive substances attached on the fiber. The
extractives are hemicellulose and lignin. Hemicellulose is one of the plant tissue that serves as water
reserves. This network of hemicellulose is made up of clusters of double and branched
polysaccharides. Lignin is a support network of plants and protects plants from the surrounding
environment. Lignin acts as a matrix to plants and has thermoplastic properties that are not readily
biodegradable by water or other compounds. The alkali treatment of natural fibers aims to defibrillate
and reduce impurities on the fiber surface [4]. The cellulose is a new material that can be used as an
reinforcement in the polymer [5]. With the addition of cellulose from SMF to polymer is expected to
improve the composite strength. The process of isolating cellulose by chemical treatment is to soak the
SMF in a solution of Sodium hydroxide followed by immersion in hydrogen peroxide. The results of
subsequent chemical treatments will be characterized by testing of chemical composition, scanning
electron microscopy (SEM), Fourier transform infrared (FTIR) and X-ray diffraction (XRD).
2. Experimental
2.1. Material
Salacca midrib fibers were obtained from Turi, Sleman, Daerah Istimewa Yogyakarta, Indonesia.
Sodium hydroxide (NaOH) with a purity of 99% and Hydrogen peroxide (H2O2) with a purity of 3%.
2.2. Isolation and chemical analysis of cellulose
SMF were separated from the bast, then dried at the temperature 50ยฐC for 36 hours, the chemical
composition of ฮฑ-cellulose and holocellulose was determined by chlorite acid modification method
and lignin refers to SNI 0492:2008. The fibers were immersed in 2% wt. of NaOH solution [6] at the
temperature 70ยฐC for 120 minute at atmospheric pressure and then continuing by bleaching treatment
with 3% (v/v) of hydrogen peroxide solution at temperature 60ยฐC, PH10, for 60 minute [7].
2.3. Characterization
The morphology of each stage of chemical treatment on SMF fibers is seen using SEM model JEOLโ€“
JSM 6510LA operated at 15 kV. The samples were coated with Au using the sputtering technique.
Stages of chemical treatment performed are alkalization and bleaching. Supporting data ensuring that
fibers are clean from impurity or other extractive substances require FTIR testing. FTIR aims to
detected the functional group, the FTIR model is Shimadzu operate in the range of 400-4000 cm-1.
The XRD aims to identify the structure of fiber. The XRD model is Rigaku Miniflex600 operating
with Cu Kฮฑ radiation (ฮป=1.5418 ร…) ranging from 2ฮธ = 4ยฐ - 40ยฐ. The Crystallinity index can be
calculated using the segal method [8] as shown in Eq. (1):
CrI =
(I002 โˆ’ Iamorph)
I002
x 100% (1)
3
1234567890โ€˜โ€™โ€œโ€
3rd Annual Applied Science and Engineering Conference (AASEC 2018) IOP Publishing
IOP Conf. Series: Materials Science and Engineering 434 (2018) 012078 doi:10.1088/1757-899X/434/1/012078
Generally the maximum peak intensity located at 2theta = 22ยฐ which represent the crystalline
cellulose. Iamorph is the valley intensity (minimum) located at 2 theta is around 18ยฐ which represent
amorphous cellulose.
3. Results and Discussion
3.1. Chemical analysis and morphology
The purpose of purification process was to separate the cellulose fibers by removed lignin and other
extractives. Table 1 shows the purified process of cellulose from SMF. Table 1 shows that the lowest
percentage of ฮฑ-cellulose and the raw fiber has the highest percentage of hemicellulose and lignin.
After purification processes indicated that increasing ฮฑ-cellulose content from raw fibers 47.18%,
alkali 49.14%, and bleached 51.81%. The effect of the different chemical treatments shown in Figure
2. from the change colour of fibers. The bleaching process conducted after the alkali treatment step
contributed to modifying the fiber color because it removed the lignin. Figure 3 shows the SEM
images of the raw SMF compare by the chemical purified cellulose fibers. After chemical
pretreatment, the cellulose fibers were defibrillation into individual micro sized fibers.
Figure 2. Optical photographs showing the different chemical treatments a)
untread SMF, b) alkali treated, c) bleached fibers.
Table 1. Chemical composition of fibers at each
stages of treatment
Material
Alpha-
Cellulose
(%)
Hemicellulose
(%)
Lignin
(%)
Raw SMF 47,18 31,89 22,27
Alkali 49,14 19,76 20.48
Bleached 51,81 23,12 18.83
Figure 3. SEM images of the a) untreated SMF and b) bleached fiber.
4
1234567890โ€˜โ€™โ€œโ€
3rd Annual Applied Science and Engineering Conference (AASEC 2018) IOP Publishing
IOP Conf. Series: Materials Science and Engineering 434 (2018) 012078 doi:10.1088/1757-899X/434/1/012078
3.2. FTIR analysis
Infrared measurements were performed on chemically treated fibers to follow the removal of
impurities material. Figure 4 compares the FTIR spectra of raw SMF fibers, alkalization and bleached
treatments. The band approximately at 1735 cmโˆ’1 in the spectrum of raw SMF is attributed to Cโ•O
stretching of the acetyl and uronic ester groups of hemicellulose. The band approximately at 1512
cmโˆ’1 that could be seen in the spectrum recorded for raw SMF was ascribed to the aromatic Cโ•C
stretching from the aromatic ring of lignin [1] [9]. Lignin presented characteristic at the other band in
the range 1250โ€“1319 cmโˆ’1 indicate that stretching of acetyl C-O and aromatic skeletal vibration CH2
Wagging (lignin). The band located at 1635 O-H (water content).
Figure 4. FTIR spectra of fibers at each stage of treatment.
3.3. XRD analysis
The x-ray diffractogram of the raw SMF, alkali, and bleached treatments are shown in Figure 5.
Calculation of the crystallinity index based on the Equation 1. For all samples showed that crystalline
structure of cellulose 1 in the major intensity peak 2ฮธ around 22.6ยฐ, with the intensity of amorphous
region peak at a 2ฮธ around 18ยฐ [1]. The crystallinity indices increasing from 62,4% for raw fibers,
alkali 69.55%, and bleached 70.04%. During the step of purification (raw SMF-alkali-bleaching)
progressively increasing the crystallinity index of fiber. This was considered to the progressive
removal of amorphous material.
Figure 5. XRD Diffractogram of each stages of chemical treatment.
5
1234567890โ€˜โ€™โ€œโ€
3rd Annual Applied Science and Engineering Conference (AASEC 2018) IOP Publishing
IOP Conf. Series: Materials Science and Engineering 434 (2018) 012078 doi:10.1088/1757-899X/434/1/012078
4. Conclusions
Salacca midrib fibers as a new source of renewable materials contained ฮฑ-cellulose has been isolated
with the yield of 51,81%. The crystallinity index of the cellulose has been extracted with the yield of
70,04%. Effective isolation of cellulose in salacca midrib fibers has been demonstrated by alkalization
and bleaching treatment. We have successfully increase content of ฮฑ-cellulose and decrease amount of
non-cellulosic content by chemical treatment using 2% NaOH at the temperature of 70ยฐC for 120 min
and bleaching with 3% of H2O2 at the temperature of 60ยฐC for 60 min with PH 10.
Acknowledgments
This experimental was supported by Research Grant of Graduate Program (Cont.No.
1795/UN1/DITLIT/DIT-LIT/LT/2018), Universitas Gadjah Mada. The authors are also grateful to the
staff of Laboratory of Engineering Material, Department of Mechanical and Industrial Engineering,
Faculty of Engineering, Universitas Gadjah Mada.
References
[1] Sheltami R M, Abdullah I, Ahmad I, Dufresne A and Kargarzadeh H 2012 Extraction of
cellulose nanocrystals from mengkuang leaves (Pandanus tectorius) Carbohydrate
Polymers 88(2) 772-779
[2] Kaushik A and Singh M 2011 Isolation and characterization of cellulose nanofibrils from wheat
straw using steam explosion coupled with high shear homogenization Carbohydrate
research 346(1) 76-85
[3] S Darmanto, H S B Rochardjo, Jamasri and R Widyorini 2017 Effects of Steaming and Steam
Explosion on Mechanical Properties of Snake Fruit (Salacca) Fiber International Journal of
Engineering and Technology (IJET) 9 pp. 150-157
[4] M Li, S Zhou and X Guo 2017 Effects of alkali-treated bamboo fibers on the morphology and
mechanical properties of oil well cement Construction and Building Materials 150 pp. 619-
625
[5] Ng H M, Sin L T, Tee T T, Bee S T, Hui D, Low C Y and Rahmat A R 2015 Extraction of
cellulose nanocrystals from plant sources for application as reinforcing agent in
polymers Composites Part B: Engineering 75 176-200
[6] Darmanto S, Rochardjo H S, Jamasri and Widyorini R 2017 Effects of alkali and steaming on
mechanical properties of snake fruit (Salacca) fiber AIP Conference Proceedings 1788(1),
p. 030060)
[7] Yudhanto F and Rochardjo H S 2018 Application of taguchi method for selection parameter
bleaching treatments against mechanical and physical properties of agave cantala fiber
In IOP Conference Series: Materials Science and Engineering 352(1) pp. 012002 IOP
Publishing
[8] Segal, L G J M A, Creely J J, Martin Jr A E and Conrad C M 1959 An empirical method for
estimating the degree of crystallinity of native cellulose using the X-ray diffractometer
Textile Research Journal 29(10) 786-794
[9] Chen W, Yu H, Liu Y, Hai Y, Zhang M and Chen P 2011 Isolation and characterization of
cellulose nanofibers from four plant cellulose fibers using a chemical-ultrasonic process
Cellulose 18(2) 433-442

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Open access proceedings journal of physics conference series iop

  • 1. IOP Conference Series: Materials Science and Engineering PAPER โ€ข OPEN ACCESS Isolation of cellulose from salacca midrib fibers by chemical treatments To cite this article: V Yudha et al 2018 IOP Conf. Ser.: Mater. Sci. Eng. 434 012078 View the article online for updates and enhancements. This content was downloaded from IP address 202.43.95.72 on 05/12/2018 at 03:59
  • 2. 1 Content from this work may be used under the terms of the Creative Commons Attribution 3.0 licence. Any further distribution of this work must maintain attribution to the author(s) and the title of the work, journal citation and DOI. Published under licence by IOP Publishing Ltd 1234567890โ€˜โ€™โ€œโ€ 3rd Annual Applied Science and Engineering Conference (AASEC 2018) IOP Publishing IOP Conf. Series: Materials Science and Engineering 434 (2018) 012078 doi:10.1088/1757-899X/434/1/012078 Isolation of cellulose from salacca midrib fibers by chemical treatments V Yudha1 , H S B Rochardjo1* , J Jamasri1 , R Widyorini4 , F Yudhanto1,2 and S Darmanto1,3 1 Department of Mechanical and Industrial Engineering, Universitas Gadjah Mada, 55284 Yogyakarta, Indonesia 2 Department of Mechanical Engineering, Universitas Muhammadiyah Yogyakarta, 55183 Yogyakarta, Indonesia 3 Department of Industrial Engineering, Vocation School, Universitas Diponegoro, Semarang, Indonesia 4 Department of Forest Product Technology, Universitas Gadjah Mada, 55281 Yogyakarta, Indonesia *heru-sbr@ugm.ac.id Abstract. Salacca midrib fibers (SMF) have potential as a new source of cellulosic material. The method of isolate cellulose from SMF carried out by the different stages of chemical treatment. First stage is alkalization using sodium hydroxide and then second stage is bleaching treatment using hydrogen peroxide. The chemical composition analysis of SMF was determined at different stages of chemical treatments. Physical analysis was carried out by fourier transform infrared spectroscopy (FTIR) and x-ray diffraction (XRD). Change in surface morphologies of fibers were characterized by scanning electron microscopy (SEM). Isolation process of cellulose from SMF by alkali and bleaching treatments successfully increased content of ฮฑ-cellulose, decreased content of lignin and increased percentage of index crystallinity of fibers. 1. Introduction Natural fibers can be grouped based on the source that comes from plants, animals or minerals. The natural fibers of the cultivated plants have the advantage of obtaining and having a shorter harvest time. Lignocellulosic fibers, also known as cellulose-based fibers, can be devide into nonwood and wood or plants fiber. Natural fibers are an alternative reinforcement for composite application due to the environmental issues [1]. The main content of natural fibers is cellulose, hemicellulose and lignin [2]. Cellulose is renewable, biodegradable and the most abundant natural polymer. Salacca midrib fibers (SMF) is one of prospective tropical plants to produce fibers from their bast (figure. 1). SMF has a diameter of 3 to 3,5 cm with a length of 110 cm. The fibers extracted from the bast of salacca midrib are generally 4-5 years old The chemical composition of raw SMF contain ฮฑ-cellulose 47.18%, hemicellulose 31.89%, and lignin 22.27% [3].
  • 3. 2 1234567890โ€˜โ€™โ€œโ€ 3rd Annual Applied Science and Engineering Conference (AASEC 2018) IOP Publishing IOP Conf. Series: Materials Science and Engineering 434 (2018) 012078 doi:10.1088/1757-899X/434/1/012078 Figure 1. Salacca midrib fibers. The isolation proses to separate the cellulose from the extractive substances attached on the fiber. The extractives are hemicellulose and lignin. Hemicellulose is one of the plant tissue that serves as water reserves. This network of hemicellulose is made up of clusters of double and branched polysaccharides. Lignin is a support network of plants and protects plants from the surrounding environment. Lignin acts as a matrix to plants and has thermoplastic properties that are not readily biodegradable by water or other compounds. The alkali treatment of natural fibers aims to defibrillate and reduce impurities on the fiber surface [4]. The cellulose is a new material that can be used as an reinforcement in the polymer [5]. With the addition of cellulose from SMF to polymer is expected to improve the composite strength. The process of isolating cellulose by chemical treatment is to soak the SMF in a solution of Sodium hydroxide followed by immersion in hydrogen peroxide. The results of subsequent chemical treatments will be characterized by testing of chemical composition, scanning electron microscopy (SEM), Fourier transform infrared (FTIR) and X-ray diffraction (XRD). 2. Experimental 2.1. Material Salacca midrib fibers were obtained from Turi, Sleman, Daerah Istimewa Yogyakarta, Indonesia. Sodium hydroxide (NaOH) with a purity of 99% and Hydrogen peroxide (H2O2) with a purity of 3%. 2.2. Isolation and chemical analysis of cellulose SMF were separated from the bast, then dried at the temperature 50ยฐC for 36 hours, the chemical composition of ฮฑ-cellulose and holocellulose was determined by chlorite acid modification method and lignin refers to SNI 0492:2008. The fibers were immersed in 2% wt. of NaOH solution [6] at the temperature 70ยฐC for 120 minute at atmospheric pressure and then continuing by bleaching treatment with 3% (v/v) of hydrogen peroxide solution at temperature 60ยฐC, PH10, for 60 minute [7]. 2.3. Characterization The morphology of each stage of chemical treatment on SMF fibers is seen using SEM model JEOLโ€“ JSM 6510LA operated at 15 kV. The samples were coated with Au using the sputtering technique. Stages of chemical treatment performed are alkalization and bleaching. Supporting data ensuring that fibers are clean from impurity or other extractive substances require FTIR testing. FTIR aims to detected the functional group, the FTIR model is Shimadzu operate in the range of 400-4000 cm-1. The XRD aims to identify the structure of fiber. The XRD model is Rigaku Miniflex600 operating with Cu Kฮฑ radiation (ฮป=1.5418 ร…) ranging from 2ฮธ = 4ยฐ - 40ยฐ. The Crystallinity index can be calculated using the segal method [8] as shown in Eq. (1): CrI = (I002 โˆ’ Iamorph) I002 x 100% (1)
  • 4. 3 1234567890โ€˜โ€™โ€œโ€ 3rd Annual Applied Science and Engineering Conference (AASEC 2018) IOP Publishing IOP Conf. Series: Materials Science and Engineering 434 (2018) 012078 doi:10.1088/1757-899X/434/1/012078 Generally the maximum peak intensity located at 2theta = 22ยฐ which represent the crystalline cellulose. Iamorph is the valley intensity (minimum) located at 2 theta is around 18ยฐ which represent amorphous cellulose. 3. Results and Discussion 3.1. Chemical analysis and morphology The purpose of purification process was to separate the cellulose fibers by removed lignin and other extractives. Table 1 shows the purified process of cellulose from SMF. Table 1 shows that the lowest percentage of ฮฑ-cellulose and the raw fiber has the highest percentage of hemicellulose and lignin. After purification processes indicated that increasing ฮฑ-cellulose content from raw fibers 47.18%, alkali 49.14%, and bleached 51.81%. The effect of the different chemical treatments shown in Figure 2. from the change colour of fibers. The bleaching process conducted after the alkali treatment step contributed to modifying the fiber color because it removed the lignin. Figure 3 shows the SEM images of the raw SMF compare by the chemical purified cellulose fibers. After chemical pretreatment, the cellulose fibers were defibrillation into individual micro sized fibers. Figure 2. Optical photographs showing the different chemical treatments a) untread SMF, b) alkali treated, c) bleached fibers. Table 1. Chemical composition of fibers at each stages of treatment Material Alpha- Cellulose (%) Hemicellulose (%) Lignin (%) Raw SMF 47,18 31,89 22,27 Alkali 49,14 19,76 20.48 Bleached 51,81 23,12 18.83 Figure 3. SEM images of the a) untreated SMF and b) bleached fiber.
  • 5. 4 1234567890โ€˜โ€™โ€œโ€ 3rd Annual Applied Science and Engineering Conference (AASEC 2018) IOP Publishing IOP Conf. Series: Materials Science and Engineering 434 (2018) 012078 doi:10.1088/1757-899X/434/1/012078 3.2. FTIR analysis Infrared measurements were performed on chemically treated fibers to follow the removal of impurities material. Figure 4 compares the FTIR spectra of raw SMF fibers, alkalization and bleached treatments. The band approximately at 1735 cmโˆ’1 in the spectrum of raw SMF is attributed to Cโ•O stretching of the acetyl and uronic ester groups of hemicellulose. The band approximately at 1512 cmโˆ’1 that could be seen in the spectrum recorded for raw SMF was ascribed to the aromatic Cโ•C stretching from the aromatic ring of lignin [1] [9]. Lignin presented characteristic at the other band in the range 1250โ€“1319 cmโˆ’1 indicate that stretching of acetyl C-O and aromatic skeletal vibration CH2 Wagging (lignin). The band located at 1635 O-H (water content). Figure 4. FTIR spectra of fibers at each stage of treatment. 3.3. XRD analysis The x-ray diffractogram of the raw SMF, alkali, and bleached treatments are shown in Figure 5. Calculation of the crystallinity index based on the Equation 1. For all samples showed that crystalline structure of cellulose 1 in the major intensity peak 2ฮธ around 22.6ยฐ, with the intensity of amorphous region peak at a 2ฮธ around 18ยฐ [1]. The crystallinity indices increasing from 62,4% for raw fibers, alkali 69.55%, and bleached 70.04%. During the step of purification (raw SMF-alkali-bleaching) progressively increasing the crystallinity index of fiber. This was considered to the progressive removal of amorphous material. Figure 5. XRD Diffractogram of each stages of chemical treatment.
  • 6. 5 1234567890โ€˜โ€™โ€œโ€ 3rd Annual Applied Science and Engineering Conference (AASEC 2018) IOP Publishing IOP Conf. Series: Materials Science and Engineering 434 (2018) 012078 doi:10.1088/1757-899X/434/1/012078 4. Conclusions Salacca midrib fibers as a new source of renewable materials contained ฮฑ-cellulose has been isolated with the yield of 51,81%. The crystallinity index of the cellulose has been extracted with the yield of 70,04%. Effective isolation of cellulose in salacca midrib fibers has been demonstrated by alkalization and bleaching treatment. We have successfully increase content of ฮฑ-cellulose and decrease amount of non-cellulosic content by chemical treatment using 2% NaOH at the temperature of 70ยฐC for 120 min and bleaching with 3% of H2O2 at the temperature of 60ยฐC for 60 min with PH 10. Acknowledgments This experimental was supported by Research Grant of Graduate Program (Cont.No. 1795/UN1/DITLIT/DIT-LIT/LT/2018), Universitas Gadjah Mada. The authors are also grateful to the staff of Laboratory of Engineering Material, Department of Mechanical and Industrial Engineering, Faculty of Engineering, Universitas Gadjah Mada. References [1] Sheltami R M, Abdullah I, Ahmad I, Dufresne A and Kargarzadeh H 2012 Extraction of cellulose nanocrystals from mengkuang leaves (Pandanus tectorius) Carbohydrate Polymers 88(2) 772-779 [2] Kaushik A and Singh M 2011 Isolation and characterization of cellulose nanofibrils from wheat straw using steam explosion coupled with high shear homogenization Carbohydrate research 346(1) 76-85 [3] S Darmanto, H S B Rochardjo, Jamasri and R Widyorini 2017 Effects of Steaming and Steam Explosion on Mechanical Properties of Snake Fruit (Salacca) Fiber International Journal of Engineering and Technology (IJET) 9 pp. 150-157 [4] M Li, S Zhou and X Guo 2017 Effects of alkali-treated bamboo fibers on the morphology and mechanical properties of oil well cement Construction and Building Materials 150 pp. 619- 625 [5] Ng H M, Sin L T, Tee T T, Bee S T, Hui D, Low C Y and Rahmat A R 2015 Extraction of cellulose nanocrystals from plant sources for application as reinforcing agent in polymers Composites Part B: Engineering 75 176-200 [6] Darmanto S, Rochardjo H S, Jamasri and Widyorini R 2017 Effects of alkali and steaming on mechanical properties of snake fruit (Salacca) fiber AIP Conference Proceedings 1788(1), p. 030060) [7] Yudhanto F and Rochardjo H S 2018 Application of taguchi method for selection parameter bleaching treatments against mechanical and physical properties of agave cantala fiber In IOP Conference Series: Materials Science and Engineering 352(1) pp. 012002 IOP Publishing [8] Segal, L G J M A, Creely J J, Martin Jr A E and Conrad C M 1959 An empirical method for estimating the degree of crystallinity of native cellulose using the X-ray diffractometer Textile Research Journal 29(10) 786-794 [9] Chen W, Yu H, Liu Y, Hai Y, Zhang M and Chen P 2011 Isolation and characterization of cellulose nanofibers from four plant cellulose fibers using a chemical-ultrasonic process Cellulose 18(2) 433-442