METHOD DEVELOPMENT OF HOLOCELLULOSE ANALYSIS

• Main Author: Apriana Purwita, Chandra
• Format: Theses
• Language: Indonesia
• Subjects: Kimia
• Online Access: https://digilib.itb.ac.id/gdl/view/57289
• Institution: Institut Teknologi Bandung

Holocellulose is a carbohydrate fraction in wood and non-wood which is a combination of cellulose and hemicellulose. The holocellulose analysis method is based on lignin removal (delignification) in extractive-free raw materials. The holocellulose analysis method is very outdated and the delignification conditions need to be optimized to achieve precise separation of the lignin and carbohydrate fractions to obtain more accurate results. Therefore, it is necessary to develop a holocellulose analysis method. This study aims to develop a holocellulose analysis method by optimizing the temperature, time, and concentration of sodium chlorite in the delignification of materials and to determine and optimize the reagents that can detect the end point of delignification. The study used five types of raw materials, namely Eucalyptus pellita, Acacia mangium, Pinus merkusii, Palm Oil Empty Fruit Bunches (palm oil EFB) (Elaeis oleifera), and abaca (Musa textilis Nee). Determination and optimization of reagents to detect delignification endpoints and optimization of delignification conditions only using Eucalyptus pellita. Other raw materials are used for the analysis of the chemical components. Determination and optimization of reagents for detecting delignification end point was carried out by varying the concentration of monoethanolamine solution in 1,4- dioxane from 1 to 5%. Parameters observed were yield, lignin content, total carbohydrates, brightness, and color. The design of experiments for the optimization of delignification conditions was carried out by Design-Expert software using Response Surface Methodology (RSM) by varying the temperature, time, and sodium chlorite concentration to obtain 20 combinations treatment of Central Composite Design (CCD) and the responses observed were yield, lignin content, and total carbohydrate. The software gave the optimum prediction of the delignification conditions which are then verified through laboratory experiments. The holocellulose analysis was then carried out under optimal delignification conditions. The holocellulose fraction was then characterized by Scanning Electron Microscope (SEM), X-ray Difraction (XRD), and Fourier Transform Infrared Spectroscopy (FTIR) then compared with standard reference pulp, Eucalyptus pellita raw material, and the holocellulose fraction ASTM D1104-56 method (1978). Based on the experiment, 5% hot solution of monoethanolamine in 1,4- dioxane was effective for detecting the end point of delignification. The delignification end point was reached if the holocellulose fraction did not turn brown after being reacted with 5% hot solution of monoethanolamine in 1,4- dioxane. The optimal delignification conditions were obtained at 78 ºC, 1 hour, and 1 gram of sodium chlorite per 2 grams of raw material. Based on the characterization of the holocellulose fraction, the crystallinity index slightly increased, the surface was smoother on the SEM photo, and there was a decrease in the absorbance in the typical band of lignin and an increase in the absorbance in the typical band of cellulose indicating that the developed method has better delignification than ASTM D1104-56 (1978) so that it will produce a total summative of the chemical components of the material that is close to 100%.