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Comparative study of various pretreatment reagents on rice husk and structural changes assessment of the optimized pretreated rice husk

Ang TN, Ngoh GC, Chua AS

Bioresour Technol, 2013 May;135:116-9.
PMID: 23138072 DOI: 10.1016/j.biortech.2012.09.045

The performance of alkalis (NaOH and Ca(OH)2) and acids (H2SO4, HCl, H3PO4, CH3COOH, and HNO3) in the pretreatment of rice husk was screened, and a suitable reagent was assessed for subsequent optimization using response surface methodology. From the assessment, HCl that hydrolysed rice husk well was optimized with three parameters (HCl loading, pretreatment duration, and temperature) using Box-Behnken Design. The optimized condition (0.5% (w/v) HCl loading, 125 °C, 1.5 h) is relatively mild, and resulted in ~22.3mg TRS/ml hydrolysate. The reduced model developed has good predictability, where the predicted and experimental results differ by only 2%. The comprehensive structural characterization studies that involved FT-IR, XRD, SEM, and BET surface area determination showed that the pretreated rice husk consisted mainly of cellulose and lignin. Compared to untreated rice husk, pretreated rice husk possessed increased pore size and pore volume, which are expected to be beneficial for fungal growth during fermentation.
Fulltext Elucidation of the effect of ionic liquid pretreatment on rice husk via structural analyses

Ang TN, Ngoh GC, Chua AS, Lee MG

Biotechnol Biofuels, 2012 Sep 07;5(1):67.
PMID: 22958710 DOI: 10.1186/1754-6834-5-67

BACKGROUND: In the present study, three ionic liquids, namely 1-butyl-3-methylimidazolium chloride ([BMIM]Cl), 1-ethyl-3-methylimidazolium acetate ([EMIM]OAc), and 1-ethyl-3-methylimidazolium diethyl phosphate ([EMIM]DEP), were used to partially dissolve rice husk, after which the cellulose were regenerated by the addition of water. The aim of the investigation is to examine the implications of the ionic liquid pretreatments on rice husk composition and structure.
RESULTS: From the attenuated total reflectance Fourier transform-infrared (ATR FT-IR) spectroscopy, X-ray diffraction (XRD) and scanning electron microscopy (SEM) results, the regenerated cellulose were more amorphous, less crystalline, and possessed higher structural disruption compared with untreated rice husk. The major component of regenerated cellulose from [BMIM]Cl and [EMIM]DEP pretreatments was cellulose-rich material, while cellulose regenerated from [EMIM]OAc was a matrix of cellulose and lignin. Cellulose regenerated from ionic pretreatments could be saccharified via enzymatic hydrolysis, and resulted in relatively high reducing sugars yields, whereas enzymatic hydrolysis of untreated rice husk did not yield reducing sugars. Rice husk residues generated from the ionic liquid pretreatments had similar chemical composition and amorphousity to that of untreated rice husk, but with varying extent of surface disruption and swelling.
CONCLUSIONS: The structural architecture of the regenerated cellulose and rice husk residues showed that they could be used for subsequent fermentation or derivation of cellulosic compounds. Therefore, ionic liquid pretreatment is an alternative in the pretreatment of lignocellulosic biomass in addition to the conventional chemical pretreatments.
Oxidative hydrothermal surface modification of activated carbon for sevoflurane removal

Ang TN, Young BR, Burrell R, Taylor M, Aroua MK, Baroutian S

Chemosphere, 2021 Feb;264(Pt 2):128535.
PMID: 33045509 DOI: 10.1016/j.chemosphere.2020.128535

The emission of waste anaesthetic gas is a growing contributor to global warming and remains a factor in atmospheric ozone depletion. Volatile anaesthetics in medical waste gases could be removed via adsorption using suitable activated carbon materials possessing an enhanced affinity to anaesthetic molecules. In this work, the effects of surface physical and chemical properties on sevoflurane adsorption were investigated by oxidative hydrothermal surface modification of a commercial activated carbon using only distilled water. The hydrothermal surface modification was carried out at different treatment temperatures (150-300 °C) for varying durations (10-30 min), and adsorption was conducted under fixed conditions (bed depth = 10 cm, inlet concentration = 528 mg/L, and flow rate = 3 L/min). The hydrothermal treatment generally increased the BET surface area of the activated carbons. At oxidation temperatures above 200 °C, the micropore volume of the samples diminished. The relative amount of surface oxygen was enriched as the treatment temperature increased. Treatment duration did not significantly affect the introduction of relative amount of surface oxygen, except at higher temperatures. There were no new types of functional groups introduced. However, disappearance and re-formation of oxygen functional groups containing C-O structures (as in hydroxyl and ether groups) occurred when treatment temperature was increased from 150 to 200 °C, and when treatments were conducted above 200 °C, respectively. The ester/acetal groups were enriched under the temperature range studied. The findings suggested that the re-formation of surface oxygen functionalities might lead to the development of functional groups that improve sevoflurane adsorption.
Enrichment of surface oxygen functionalities on activated carbon for adsorptive removal of sevoflurane

Ang TN, Young BR, Taylor M, Burrell R, Aroua MK, Chen WH, et al.

Chemosphere, 2020 Dec;260:127496.
PMID: 32659541 DOI: 10.1016/j.chemosphere.2020.127496

Activated carbons have been reported to be useful for adsorptive removal of the volatile anaesthetic sevoflurane from a vapour stream. The surface functionalities on activated carbons could be modified through aqueous oxidation using oxidising solutions to enhance the sevoflurane adsorption. In this study, an attempt to oxidise the surface of a commercial activated carbon to improve its adsorption capacity for sevoflurane was conducted using 6 mol/L nitric acid, 2 mol/L ammonium persulfate, and 30 wt per cent (wt%) of hydrogen peroxide (H2O2). The adsorption tests at fixed conditions (bed depth: 10 cm, inlet concentration: 528 mg/L, and flow rate: 3 L/min) revealed that H2O2 oxidation gave desirable sevoflurane adsorption (0.510 ± 0.005 mg/m2). A parametric study was conducted with H2O2 to investigate the effect of oxidation conditions to the changes in surface oxygen functionalities by varying the concentration, oxidation duration, and temperature, and the Conductor-like Screening Model for Real Solvents (COSMO-RS) was applied to predict the interactions between oxygen functionalities and sevoflurane. The H2O2 oxidation incorporated varying degrees of both surface oxygen functionalities with hydrogen bond (HB) acceptor and HB donor characters under the studied conditions. Oxidised samples with enriched oxygen functionalities with HB acceptor character and fewer HB donor character exhibited better adsorption capacity for sevoflurane. The presence of a high amount of oxygen functional groups with HB donor character adversely affected the sevoflurane adsorption despite the enrichment of oxygen functional groups with HB acceptor character that have a higher tendency to adsorb sevoflurane.
Breakthrough analysis of continuous fixed-bed adsorption of sevoflurane using activated carbons

Ang TN, Young BR, Taylor M, Burrell R, Aroua MK, Baroutian S

Chemosphere, 2020 Jan;239:124839.
PMID: 31726519 DOI: 10.1016/j.chemosphere.2019.124839

The inhalational anaesthetic agent - sevoflurane is widely employed for the induction and maintenance of surgical anaesthesia. Sevoflurane possesses a high global warming potential that imposes negative impact to the environment. The only way to resolve the issue is to remove sevoflurane from the medical waste gas before it reaches the atmosphere. A continuous adsorption study with a fixed-bed column was conducted using two commercial granular activated carbons (E-GAC and H-GAC), to selectively remove sevoflurane. The effect of bed depth (Z, 5-15 cm), gas flow rate (Q, 0.5-6.0 L/min) and inlet sevoflurane concentration (C0, ∼55-700 mg/L) was investigated. E-GAC demonstrated ∼60% higher adsorption capacity than H-GAC under the same operating conditions. Varying the levels of Z, Q and C0 showed significant differences in the adsorption capacities of E-GAC, whereas only changing the C0 level had significant differences for H-GAC. Three breakthrough models (Adams-Bohart, Thomas, and Yoon-Nelson) and Bed-depth/service time (BDST) analysis were applied to predict the breakthrough characteristics of the adsorption tests and determine the characteristic parameters of the column. The Yoon-Nelson and Thomas model-predicted breakthrough curves were in good agreement with the experimental values. In the case of the Adams-Bohart model, a low correlation was observed. The predicted breakthrough time (tb) based on kinetic constant (kBDST) in BDST analysis showed satisfactory agreement with the measured values. The results suggest the possibility of designing, scaling up and optimising an adsorption system for removing sevoflurane with the aid of the models and BDST analysis.
Authors' response to comments on Ang et al. "Breakthrough analysis of continuous fixed-bed adsorption of sevoflurane using activated carbons"

Ang TN, Young BR, Taylor M, Burrell R, Aroua MK, Baroutian S

Chemosphere, 2020 05;247:126389.
PMID: 32147228 DOI: 10.1016/j.chemosphere.2020.126389