Ultrasound-assisted Extraction Method for Element Determination in Lignocellulosic Biomass

IF 1.1 Q4 CHEMISTRY, ANALYTICAL Brazilian Journal of Analytical Chemistry Pub Date : 2023-09-11 DOI:10.30744/brjac.2179-3425.ar-51-2023
Karen Giacobe, Débora de Almeida, Samuel Waechter, Fabio Duarte, Cezar Bizzi
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Abstract

In this work, a sample preparation method based on ultrasound-assisted extraction (UAE) for the determination of Al, Ba, Ca, Fe, K, Mg, Mn, Na, P, Sr, and Zn in lignocellulosic biomasses (sugarcane bagasse, eucalyptus wood residues, and pine wood residues) was evaluated. Reference values were achieved following the EN ISO 16967, which was based on a microwave-assisted wet digestion sample preparation method for further element determination by inductively coupled plasma optical emission spectrometry (ICP OES). The optimizations for the proposed UAE method were performed using 250 mg of sugarcane bagasse sample, where the ultrasonic bath frequency (25, 35, 37, 45, 80, and 130 kHz), and acoustic amplitude (50, 70 and 100%) were evaluated. After selecting the most efficient extractant solvent (20 mL of 1 mol L-1 of H2O2, HNO3, H2SO4, H2O, or CH2O2), the extraction temperature (20, 50, or 70 ºC) and time (15, 30, or 40 min) were evaluated. The most efficient extraction condition using the UAE method employed 45 kHz (70% amplitude), 20 mL of 1 mol L-1 of H2SO4, and 50 °C for 30 min. The optimized UAE was used for extraction and subsequent element determination in residues of pine wood and eucalyptus wood. Although poor recoveries were observed for Al, Ba, and Fe (lower than 75%), the results for Ca, K, Mg, Mn, Na, P, Sr, and Zn were in agreement (Student t-test, 95% confidence level) with those obtained by EN ISO 16967. Therefore, the proposed UAE method proved to be efficient for the determination of most of the evaluated elements in lignocellulosic biomasses with different matrix complexity, employing milder extraction conditions and diluted reagents.
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超声辅助提取法测定木质纤维素生物质中元素
本文研究了一种基于超声辅助提取(UAE)的样品制备方法,用于测定木质纤维素生物质(甘蔗甘蔗渣、桉树木渣和松木渣)中Al、Ba、Ca、Fe、K、Mg、Mn、Na、P、Sr和Zn的含量。参照EN ISO 16967标准,采用微波辅助湿消解样品制备方法,通过电感耦合等离子体光学发射光谱法(ICP OES)进一步测定元素。采用250 mg甘蔗渣样品,对超声浴频率(25、35、37、45、80和130 kHz)和声波振幅(50、70和100%)进行了优化。选择最有效的萃取溶剂(1 mol L-1的H2O2、HNO3、H2SO4、H2O或CH2O2各20 mL)后,评估萃取温度(20、50或70℃)和时间(15、30或40 min)。最有效的提取条件为45 kHz(70%振幅)、20 mL (1 mol L-1) H2SO4、50°C、30 min。优化后的UAE用于松木和桉木残留物的提取和随后的元素测定。虽然观察到Al, Ba和Fe的回收率较低(低于75%),但Ca, K, Mg, Mn, Na, P, Sr和Zn的结果与EN ISO 16967获得的结果一致(学生t检验,95%置信水平)。因此,采用较温和的提取条件和稀释的试剂,所提出的UAE方法可以有效地测定不同基质复杂性的木质纤维素生物质中大多数被评价的元素。
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CiteScore
1.60
自引率
14.30%
发文量
46
期刊介绍: BrJAC is dedicated to the diffusion of significant and original knowledge in all branches of Analytical Chemistry, and is addressed to professionals involved in science, technology and innovation projects at universities, research centers and in industry.
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