Characterization of Nanocrystalline Cellulose Isolated from Empty Fruit Bunch Using Acid Hydrolysis

2017 ◽  
Vol 264 ◽  
pp. 9-12 ◽  
Author(s):  
Pei Gie Gan ◽  
Sung Ting Sam ◽  
Muhammad Faiq bin Abdullah ◽  
Nik Noriman bin Zulkepli ◽  
Yin Fong Yeong
Keyword(s):  
Acid Hydrolysis ◽  
Nanocrystalline Cellulose ◽  
Cellulose Content ◽  
Empty Fruit Bunch ◽  
X Ray Diffraction ◽  
Spectra Analysis ◽  
X Ray ◽  
Pre Treatment ◽  
High Cellulose

In recent years, there has been a great interest in the production of nanocrystalline cellulose (NCC) due to its excellent properties. In this study, empty fruit bunch (EFB) was used as the material for the production of NCC due to its high cellulose content, inexpensive and readily-available source. NCC was prepared using acid hydrolysis at 62% for 1 hours. The morphology of NCC was determined by Field Emission Scanning Electron Microscopy (FESEM). The size of NCC was less than 50 nm in width. The obtained NCC was also characterized by Fourier transform infrared spectroscopy (FTIR) and X-ray diffraction (XRD). FTIR spectra analysis showed that hemicellulose and lignin were mostly removed from the EFB after bleaching and alkaline pre-treatment. XRD diffractograms revealed that EFB nanocellulose showed a crystallinity improvement of 24.3% compared to raw EFB cellulose.

scholarly journals Characterization of cellulose nanocrystalline isolated from banana peduncles using acid hydrolysis

2021 ◽  
Vol 922 (1) ◽  
pp. 012072
Author(s):  
Ratna ◽  
S Aprilia ◽  
N Arahman ◽  
A A Munawar
Keyword(s):  
Molecular Structure ◽  
Acid Hydrolysis ◽  
Acid Concentration ◽  
Sulfuric Acid Concentration ◽  
Sulfamic Acid ◽  
Nanocrystalline Powder ◽  
Cellulose Content ◽  
X Ray Diffraction ◽  
X Ray

Abstract The study aimed to characterize cellulose nanocrystalline (NCCs) from banana peduncles using acid hydrolysis. The NCCs isolation process was done by hydrolysis using H2SO4 with concentrations of 1M, 2M, and 3M at a microwave power of 100 Watts within 1 hour of hydrolysis. The product of NCCs was characterized in term of yield, chemical composition (by FTIR), and its crystallinity. The result showed that the highest yield of 88.33% was obtained in acid hydrolysis at the concentration of 1M H2SO4. The results of the FTIR test showed that non-cellulose content had been removed and demonstrated that the molecular structure of cellulose does not change even when treated at different acid concentrations. X-Ray Diffraction analysis showed that crystallinity decreased by increasing the sulfamic acid concentration. The thermogravimetric analysis confirmed the heat resistance analysis and showed that the NCCs is gradually decomposed at a temperature range of 268.3–415.25 ¼C. The colour of cellulose nanocrystalline powder darkens as the sulfuric acid concentration increases.

Preparation and Characterization of Kenaf and Oil Palm Nanocellulose by Acid Hydrolysis Method

2020 ◽  
Vol 1010 ◽  
pp. 495-500
Author(s):  
Nurfarah Aini Mocktar ◽  
Mohammad Khairul Azhar Abdul Razab ◽  
An'amt Mohamed Noor ◽  
Nor Hakimin Abdullah
Keyword(s):  
Surface Morphology ◽  
Acid Hydrolysis ◽  
Oil Palm ◽  
Crystallinity Index ◽  
Phase Identification ◽  
X Ray Diffraction ◽  
X Ray ◽  
Hydrolysis Method ◽  
High Degree

Acid hydrolysis method become one of the attention among researcher to produce high degree nanocellulose. Integration of sonication process was used to stir and mix particles in an element for different stages. This paper revealed the surface morphology and crystallinity index of two organic plant that were kenaf and oil palm nanocellulose. Characterization of the nanocellulose were identified by 2 techniques; (1) field emission scanning electron microscope (FESEM) that provides surface morphology and elemental information of the element, (2) x-ray diffraction (XRD) for phase identification of materials crystallinity. The result showed that the properties of nanocellulose increase after sonication method have been integrated.

X-Ray Diffraction Patterns of Oil Palm Empty Fruit Bunch Fibers with Varying Crystallinity

2015 ◽  
Vol 1087 ◽  
pp. 321-328 ◽  
Author(s):  
Fatin Afifah Ahmad Kuthi ◽  
Khairiah Haji Badri ◽  
Azlin Mohmad Azman
Keyword(s):  
Acid Hydrolysis ◽  
Oil Palm ◽  
Empty Fruit Bunch ◽  
X Ray Diffraction ◽  
Xrd Pattern ◽  
X Ray ◽  
Before And After ◽  
Different Temperatures ◽  
Diffraction Patterns ◽  
Xrd Patterns

Crystallinity of oil palm fiber from empty fruit bunch (EFB) with and without tretaments was studied by analyzing the X-ray diffraction (XRD) pattern. In this paper, we focused on the effect of acid hydrolysis onto EFB on the crystallinity of the extracted cellulose. The reaction was carried out by soaking EFB in 1% (v/v) aqueous sulfuric acid (H2SO4) at different temperatures of 120, 130 and 140°C for 1 h. The XRD patterns significantly showed changes in the 2θ peaks before and after the treatment. These changes were described in term of polymorphs type present, reflection and allomorphs of the samples. XRD peak high and XRD deconvolution methods were used to calculate and compare the percentage of crystallinity of untreated EFB (UT-EFB) and acid hydrolyzed samples (AH-EFB). Based on the calculation, increment of about 1.3 times and 1.5 times were achieved by using WAXS and XRD deconvolution methods respectively. This is due to the removal of amorphous part contributed by lignin, hemicellulose and cellulose. Fourier Transform infrared (FTIR) spectra showed the presence of similar peaks in AH-EFB and commercial microcrystalline cellulose (C-MCC) at 1427, 1315, 895 and 1022 cm-1. The micrographic features showed the acid hydrolysis had successfully took place and separated the EFB microfibrils bundles.

scholarly journals Synthesis and Characterization of ZnO-SiO2 Composite Using Oil Palm Empty Fruit Bunch as a Potential Silica Source

Molecules ◽  
2021 ◽  
Vol 26 (4) ◽  
pp. 1061
Author(s):  
Fida’i Rahmat ◽  
Yap Wing Fen ◽  
Muhammad Fahmi Anuar ◽  
Nur Alia Sheh Omar ◽  
Mohd Hafiz Mohd Zaid ◽  
...  
Keyword(s):  
Oil Palm ◽  
Optical Materials ◽  
Empty Fruit Bunch ◽  
X Ray Diffraction ◽  
Structural And Optical Properties ◽  
Solid State Method ◽  
X Ray ◽  
Silica Source ◽  
Vis Spectroscopy

In this paper, the structural and optical properties of ZnO-SiO2-based ceramics fabricated from oil palm empty fruit bunch (OPEFB) were investigated. The OPEFB waste was burned at 600, 700 and 800 °C to form palm ash and was then treated with sulfuric acid to extract silica from the ash. X-ray fluorescence (XRF) and X-ray diffraction (XRD) analyses confirmed the existence of SiO2 in the sample. Field emission scanning electron microscopy (FESEM) showed that the particles displayed an irregular shape and became finer after leaching. Then, the solid-state method was used to produce the ZnO-SiO2 composite and the samples were sintered at 600, 800, 1000, 1200 and 1400 °C. The XRD peaks of the Zn2SiO4 showed high intensity, which indicated high crystallinity of the composite. FESEM images proved that the grain boundaries were larger as the temperature increased. Upon obtaining the absorbance spectrum from ultraviolet–visible (UV–Vis) spectroscopy, the energy band gaps obtained were 3.192, 3.202 and 3.214 eV at room temperature, 600 and 800 °C, respectively, and decreased to 3.127, 2.854 and 2.609 eV at 1000, 1200 and 1400 °C, respectively. OPEFB shows high potential as a silica source in producing promising optical materials.

scholarly journals Characterization of cellulose and sugarcane (Saccharum spp.) straw from five cultivars grown in the humid tropic of Mexico

2021 ◽  
Author(s):  
Liliana Yanet López-Velázquez ◽  
Sergio Salgado-García ◽  
Samuel Cordova-Sánchez ◽  
Cintya Valerio-Cardenas ◽  
Gloria Ivette Bolio-Lopez ◽  
...  
Keyword(s):  
Crystal Size ◽  
Paper Industry ◽  
Optical Microscope ◽  
Cellulose Content ◽  
X Ray Diffraction ◽  
Saccharum Spp ◽  
X Ray ◽  
Potential Source ◽  
Sugarcane Straw

Objective: The aim of this study was to determine the cellulose content and characteristics of sugarcane straw from the cultivars MEX 69-290, MEX 68-P-23, CO-997, SP 70-1284 and CP 72-2086. Design/methodology/approach: A completely random experimental design with six replicates was conducted; the study factor was the sugarcane straw from the five evaluated cultivars. For cellulose extraction, the sodium hydroxide (soda) method was used on dried sugarcane straw of 2 mm. The crystallinity and crystal size were determined with x-ray diffraction (XRD); the fiber length had achieved a measurement with a DMRE optical microscope.   Results: Among the results, it can be noted that the cultivars MEX 69-290 and SP 70-1284, which presented less cellulose content (8.4 g and 8.5 g) and lower yields (42.1% and 42.6%), while the cultivar CO-997, presented higher cellulose content and yield which ranged from 9.8 g to 49.8%. The crystallinity of cellulose was higher in the sugarcane straw from the cultivars SP 70-1284 and MEX 68-P23. The crystal size of cellulose was 2.3 nm. The length of cellulose fibers was small (<945.7 µm). Study limitations/implications: The collection of samples in the field, as well as selected materials for digestion. Findings/conclusions: The sugarcane straw is a potential source of cellulose for the paper industry.  

scholarly journals Preparation of Microcrystalline Cellulose from Oil Palm Empty Fruit Bunch Fibre Using Steam-Assisted Acid Hydrolysis

2021 ◽  
Vol 81 (1) ◽  
pp. 88-98
Author(s):  
Fatiha Ismail ◽  
Nur Eliyanti Ali Othman ◽  
Noorshamsiana Abdul Wahab ◽  
Fazliana Abdul Hamid ◽  
Astimar Abdul Aziz
Keyword(s):  
Thermal Stability ◽  
Acid Hydrolysis ◽  
Microcrystalline Cellulose ◽  
Crystallinity Index ◽  
Steam Treatment ◽  
Empty Fruit Bunch ◽  
X Ray Diffraction ◽  
X Ray ◽  
Thermal Stability Of ◽  
Scanning Electron

The isolation of microcrystalline cellulose (MCC) from empty fruit bunch fibre (EFB-fibre) using acid hydrolysis through steam treatment (autoclave) followed by ultrasonication has been successfully established. The important parameter studied was the concentration of sulphuric acid (5%, 15% and 25%) at variable fixed reaction time and temperature. The resulting MCC was characterized using FTIR, TGA, XRD and SEM. FTIR transmission at 1163 cm-1 confirmed that the structure of cellulose was retained after undergoing acid hydrolysis. Thermal stability of MCC increased after being treated with H2SO4, which was determined using TG analysis. The morphological features were identified using Scanning Electron microscope (SEM), which showed the diameters of MCC to be in the range of 10 to 200 µm. The structural property of MCC was studied using X-ray diffraction (XRD) and the results showed that the MCC produced has crystallinity index of 72%. The results revealed that the parameters used tend to influence the physicochemical properties of MCC produced. Therefore, the MCC isolated from EFB fibres will be used as precursor for future EFB derived nanocellulose as well as a promising subject in nanocomposite research.

The Use of Advanced Analytical Techniques for Characterization of the Chemical, Physical, and Crystallographic Nature of a Surface

1973 ◽  
Vol 31 ◽  
pp. 132-133 ◽  
Author(s):  
R. E. Herfert
Keyword(s):  
Surface Characterization ◽  
Analytical Techniques ◽  
X Ray Diffraction ◽  
Depth Of Penetration ◽  
X Ray ◽  
The Past ◽  
Transmission Electron ◽  
Scanning Electron

Studies of the nature of a surface, either metallic or nonmetallic, in the past, have been limited to the instrumentation available for these measurements. In the past, optical microscopy, replica transmission electron microscopy, electron or X-ray diffraction and optical or X-ray spectroscopy have provided the means of surface characterization. Actually, some of these techniques are not purely surface; the depth of penetration may be a few thousands of an inch. Within the last five years, instrumentation has been made available which now makes it practical for use to study the outer few 100A of layers and characterize it completely from a chemical, physical, and crystallographic standpoint. The scanning electron microscope (SEM) provides a means of viewing the surface of a material in situ to magnifications as high as 250,000X.

High Resolution Replication of Organoclay Surfaces

1982 ◽  
Vol 40 ◽  
pp. 576-577
Author(s):  
W. W. Barker ◽  
W. E. Rigsby ◽  
V. J. Hurst ◽  
W. J. Humphreys
Keyword(s):  
Clay Mineral ◽  
Organic Molecule ◽  
Organic Molecules ◽  
X Ray Diffraction ◽  
Xrd Pattern ◽  
X Ray ◽  
Naturally Occurring ◽  
Silicate Layers ◽  
Mineral Identification

Experimental clay mineral-organic molecule complexes long have been known and some of them have been extensively studied by X-ray diffraction methods. The organic molecules are adsorbed onto the surfaces of the clay minerals, or intercalated between the silicate layers. Natural organo-clays also are widely recognized but generally have not been well characterized. Widely used techniques for clay mineral identification involve treatment of the sample with H2 O2 or other oxidant to destroy any associated organics. This generally simplifies and intensifies the XRD pattern of the clay residue, but helps little with the characterization of the original organoclay. Adequate techniques for the direct observation of synthetic and naturally occurring organoclays are yet to be developed.

Synthesis and characterization of TiN / Ti / AISI 410 coatings

2018 ◽  
Vol 2 (1) ◽  
pp. 7
Author(s):  
S Chirino ◽  
Jaime Diaz ◽  
N Monteblanco ◽  
E Valderrama
Keyword(s):  
Synthesis And Characterization ◽  
Photoemission Spectroscopy ◽  
X Ray Diffraction ◽  
X Ray ◽  
Columnar Grains ◽  
Tin Thin Films ◽  
Steel Aisi ◽  
Interacting Surfaces ◽  
Stainless Steel Aisi

The synthesis and characterization of Ti and TiN thin films of different thicknesses was carried out on a martensitic stainless steel AISI 410 substrate used for tool manufacturing. The mechanical parameters between the interacting surfaces such as thickness, adhesion and hardness were measured. By means of the scanning electron microscope (SEM) the superficial morphology of the Ti/TiN interface was observed, finding that the growth was of columnar grains and by means of EDAX the existence of titanium was verified.  Using X-ray diffraction (XRD) it was possible to observe the presence of residual stresses (~ -3.1 GPa) due to the different crystalline phases in the coating. Under X-ray photoemission spectroscopy (XPS) it was possible to observe the molecular chemical composition of the coating surface, being Ti-N, Ti-N-O and Ti-O the predominant ones.

Studies on the Preparation, Characterization and Solubility of -Cyclodextrin-Roxythromycin Inclusion Complexes

2009 ◽  
Vol 2 (2) ◽  
pp. 523-530
Author(s):  
D. Nagasamy Venkatesh ◽  
S. Karthick ◽  
M. Umesh ◽  
G. Vivek ◽  
R.M. Valliappan ◽  
...  
Keyword(s):  
Dissolution Rate ◽  
Inclusion Complexes ◽  
Phase Solubility ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Ir Studies ◽  
Poorly Soluble ◽  
Poorly Soluble Drug

Roxythromycin/ β-cyclodextrin (Roxy/ β-CD) dispersions were prepared with a view to study the influence of β-CD on the solubility and dissolution rate of this poorly soluble drug. Phase-solubility profile indicated that the solubility of roxythromycin was significantly increased in the presence of β-cyclodextrin and was classified as AL-type, indicating the 1:1 stoichiometric inclusion complexes. Physical characterization of the prepared systems was carried out by differential scanning calorimetry (DSC), X-ray diffraction studies (XRD) and IR studies. Solid state characterization of the drug β-CD binary system using XRD, FTIR and DSC revealed distinct loss of drug crystallinity in the formulation, ostensibly accounting for enhancement of dissolution rate.

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