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Factorial design of experiments for extraction and screening analysis of organic compounds in hydrochar and its process water of sugar cane bagasse and vinasse

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Abstract

The extraction of non-volatile (NVOC), semi-volatile (SVOC), and volatile (VOC) organic compounds in water and soil samples follows well-defined protocols, already described in the specialized literature. However, for environmental matrices that are either new, complex, or difficult to define, an adaptation of the extraction procedures needs to be made. Thus, the main purpose of this paper was to find the best conditions for the extraction of NVOC, SVOC, and VOC in complex matrix samples (hydrochar-HC and process water-PW) resulting from the hydrothermal carbonization of sugar cane bagasse and vinasse. For this, a factorial design (FD) was carried out for each type of extraction and sample. Solvent and temperature were the most determining parameters for the extraction processes. The best extraction conditions for NVOC from HC were obtained using acetone, during 8 h of reflux at Soxhlet and 1.00 g of HC (50 NVOCs), while for SVOC the best conditions were those using acetone, 40 min of ultrasound, and 1.00 g of HC (50 SVOCs). For NVOC from PW, the derivatization conditions that allowed the best extraction were found at 80 °C, 30 min, and 150 μL of PW (36 NVOCs), while for SVOC, the best conditions of extraction were those using dichloromethane and 20 min in single extraction (34 SVOCs). For VOC from HC, the best conditions were 80 °C and 30 min (39 VOCs), while, from PW, these were 40 °C and 30 min (48 VOCs) of headspace equilibrium. In this way, FD enabled the adaptation of the extraction procedures for hydrochar and process water, making screening by gas chromatography-mass spectrometry (GC-MS) analysis possible.

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Funding

The authors received financial support and scholarship from the São Paulo Research Foundation—FAPESP (Grants 2005/51242-8, 2011/00574-1, 2012/23066-4, 2013/21776-7, 2014/22400-3, 2017/13230-5, 2015/22954-1, 2017/26718-6, and 2018/15733-7). M. C. B. acknowledged support from the National Council for Scientific and Technological Development—CNPq (grants 445487/2014-3 and 307925/2012-9). O. P. F. acknowledged the support from the Ceará State Foundation for Scientific and Technological Development—FUNCAP (PRONEX PR2-0101-00006.01.00/15), and from CAPES-PROCAD (Council for the Enhancement of Higher Level Personnel/Program in National Defence) 2013 Grant 183995. M. J. L. and R. C. J. S. thanked CAPES for the master scholarship received.

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Authors and Affiliations

  1. Laboratório de Estudos em Ciências Ambientais, Departamento de Química e Ciências Ambientais, Instituto de Biociências, Letras e Ciências Exatas (Ibilce), São Paulo State University (UNESP), São José do Rio Preto Campus, Sao Jose do Rio Preto, SP, 15054-000, Brazil

    Márcio Justi Laranja, Renata Cristina Júlio da Silva, Márcia Cristina Bisinoti, Altair Benedito Moreira & Camila de Almeida Melo

  2. Laboratório de Sucroquímica e Química Analítica, Departamento de Química e Ciências Ambientais, Instituto de Biociências, Letras e Ciências Exatas (Ibilce), São Paulo State University (UNESP), São José do Rio Preto Campus, Sao Jose do Rio Preto, SP, 15054-000, Brazil

    Maurício Boscolo

  3. Laboratório de Materiais Funcionais Avançados (LaMFA), Departamento de Física, Universidade Federal do Ceará (UFC), PO Box 6030, Fortaleza, Ceará, 60455-900, Brazil

    Odair Pastor Ferreira

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  1. Márcio Justi Laranja
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  2. Renata Cristina Júlio da Silva
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Correspondence to Márcio Justi Laranja or Camila de Almeida Melo.

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Laranja, M.J., da Silva, R.C.J., Bisinoti, M.C. et al. Factorial design of experiments for extraction and screening analysis of organic compounds in hydrochar and its process water of sugar cane bagasse and vinasse. Biomass Conv. Bioref. 12, 81–90 (2022). https://doi.org/10.1007/s13399-020-01035-y

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