DOI: 10.57755/t5p2-3c25
title: The effect of carbon materials addition with different specific surface areas and amount of the functional groups on the biomethane production from food waste

description: <p><span style="font-size:12px"><span lang="EN-US" style="color:rgb( 0 , 0 , 0 );font-family:&#39;times new roman&#39; , serif">Anaerobic digestion (AD) is a useful process that could be utilized for food waste (FW) management.  Previous studies have shown that carbon materials (CMs) could be an important additive for increasing biomethane yield. However, why CMs improve AD is still uncertain. A significant body of research has been dedicated to investigating the impact of CMs supplementation on biogas production. However, this article specifically emphasizes examining this effect concerning the specific surface area and the functional groups (e.g. hydroxyl groups, carbonyl groups, or unsaturated carbon structures) present on the surface of CMs, produced by torrefaction - TP (240°C/60min), pyrolysis - BC (600°C/60min), and hydrothermal carbonization - HC (240°C/60min/6-10 Bar) processes. The analyses showed that the size of the specific surface area of the CMs (TP - 7.72 m<sup>2.</sup>g<sup>-1</sup>, BC- 115.00 m<sup>2.</sup>g<sup>-1</sup>, HC - 5.46 m<sup>2.</sup>g<sup>-1</sup>), does not correspond to the production of biomethane. The highest biomethane potential was found for CMs with the lowest SSA, precisely TP and HC, equal to 407 and 394 mL<sup>.</sup>gVS<sup>-1</sup>, which was about 13 and 9% higher than production from FW as a sole source of carbon, respectively. The FTIR analysis confirmed the abundance of different organic functional groups on the surface of TP and HC, which could contribute to improved AD performance. These organic residuals, as thermal degradation products, could be an additional source of carbon for microorganisms. The addition of BC, with the highest SSA, decreased the first-order biomethane rate constant k by 16.4% in comparison to food waste without CMs, which could be related to the presence of harmful, more complex organic compounds on the surface of biochar.</span><br /></span></p>
description: <p class="MsoNormal" style="margin:0in;color:rgb( 0 , 0 , 0 );letter-spacing:normal;border:medium;font-size:12px"><strong><span lang="EN-US" style="font-size:11pt">Materials and Methods</span></strong><span lang="EN-US" style="font-size:11pt"></span></p><p class="MsoNormal" style="margin:0in;color:rgb( 0 , 0 , 0 );letter-spacing:normal;font-size:12px"><span lang="PL" style="font-size:11pt"><strong><span lang="EN-US">Carbon materials production</span></strong></span><strong><span lang="EN-US" style="font-size:11pt"></span></strong></p><p class="MsoNormal" style="margin:0in;color:rgb( 0 , 0 , 0 );letter-spacing:normal;font-size:12px"><span lang="EN-US" style="font-size:11pt">For the obtaining of CMs, wheat straw</span><span lang="PL" style="font-size:11pt"><span lang="EN-US"> harvested in central Europe, Poland has been used.</span><span lang="EN-US"> First</span></span><span lang="EN-US" style="font-size:11pt">, the substrate was </span><span lang="PL" style="font-size:11pt"><span lang="EN-US">gridded</span></span><span lang="PL" style="font-size:11pt"> </span><span lang="PL" style="font-size:11pt"><span lang="EN-US">with a laboratory</span></span><span lang="EN-US" style="font-size:11pt"> knife mill </span><span lang="PL" style="font-size:11pt"><span lang="EN-US">(</span><span lang="EN-US">32000 RPM, </span><span lang="EN-US">Chemland</span><span lang="EN-US">, Stargard, Poland)</span></span><span lang="EN-US" style="font-size:11pt"> to &lt; 1 mm particle size. </span><span lang="PL" style="font-size:11pt"><span lang="EN-US">Obtained w</span></span><span lang="EN-US" style="font-size:11pt">heat straw powder </span><span lang="PL" style="font-size:11pt"><span lang="EN-US">was</span></span><span lang="EN-US" style="font-size:11pt"> dried at 105°C for 24 h in a dr</span><span lang="PL" style="font-size:11pt"><span lang="EN-US">ying chamber</span><span lang="EN-US"> (</span></span><span lang="EN-US" style="font-size:11pt">Wamed KBC-100W</span><span lang="PL" style="font-size:11pt"><span lang="EN-US">, </span><span lang="EN-US">Warsaw, Poland)</span></span><span lang="PL" style="font-size:11pt"> </span><span lang="EN-US" style="font-size:11pt">ground and dried material </span><span lang="PL" style="font-size:11pt"><span lang="EN-US">was</span></span><span lang="EN-US" style="font-size:11pt"> used </span><span lang="PL" style="font-size:11pt"><span lang="EN-US">in 3 thermochemical processes to obtain CMs: torrefaction (240°C for 60 min), pyrolysis (</span><span lang="EN-US">600 °C for 60 min</span><span lang="EN-US">), and hydrothermal carbonization (HTC, 240°C for 60 min with pressure 6-10 bar)</span><span lang="EN-US">, </span><span lang="EN-US">the CMs that were received were named torrefied product (TP), biochar (BC), and hydrochar (HC). </span></span><span lang="EN-US" style="font-size:11pt"></span></p><p class="MsoNormal" style="margin:0in;font-size:12px"><span lang="EN-US" style="font-size:11pt">Torrefaction and pyrolysis processes were conducted in a muffle furnace (8.1/1100; SNOL, Utena, Lativa)</span><span lang="PL" style="font-size:11pt"><span lang="EN-US"> following (Stefanów et al. 2024), The dry wheat straw powder was placed into a ceramic crucible and put into a muffle furnace chamber. The furnace chamber was sealed and filled with an inert gas (CO<sub>2</sub>) flow of 2.5 dm3∙min−1 to prevent combustion. Then, the furnace was turned on; inert gas was poured into the chamber by the whole process. After the process, the furnace was turned off and left for self-cooling. Temperature was controlled by the furnace settings without a predefined heating time, while hydrothermal carbonization was conducted in the high-temperature, high-pressure reactor (Novoclave, Büchi AG, Uster, Switzerland). The reactor was heated at a rate of approximately 10°C per minute with speed mixers are set to operate at 120 rpm. For hydrochar production, 30 g of wheat straw powder was mixed with 30 g of water and placed into a hydrothermal carbonization reactor. The reactor was sealed tightly and turned on. During the process, the autogenous pressure reached 10 bars. After 60 minutes, the reactor was turned off and set for self-cooling. When the temperature dropped below 30 °C, the reactor was opened, the process gases were released by the valve, and hydrochar was collected. HC was separated from the liquid phase by vacuum filtration, Subsequently, the sample was dried in a laboratory drying chamber (Wamed KBC-100W</span><span lang="EN-US">, </span><span lang="EN-US">Warsaw, Poland)</span><span lang="EN-US"> at 105°C for 24 hours.</span></span><span lang="EN-US" style="font-size:11pt"></span></p><p class="MsoNormal" style="margin:0in;color:rgb( 0 , 0 , 0 );letter-spacing:normal;font-size:12px"><strong><span lang="PL" style="font-size:11pt"><span lang="EN-US">Anaerobic digestion process</span></span></strong><span lang="PL" style="font-size:11pt"></span><strong><span lang="EN-US" style="font-size:11pt"></span></strong></p><p class="MsoNormal" style="margin:0in;color:rgb( 0 , 0 , 0 );letter-spacing:normal;font-size:12px"><span lang="PL" style="font-size:11pt"><span lang="EN-US">Digestate used as inoculum </span><span lang="EN-US">in the</span><span lang="EN-US"> AD </span><span lang="EN-US">process was obtained from the </span><span lang="EN-US">a</span><span lang="EN-US">griculture </span><span lang="EN-US">b</span><span lang="EN-US">iogas </span><span lang="EN-US">p</span><span lang="EN-US">lant (</span><span lang="EN-US">Świdnica, Poland, Central Europe</span><span lang="EN-US">). </span><span lang="EN-US">D</span><span lang="EN-US">igestate was filtered to remove </span><span lang="EN-US">fibers </span><span lang="EN-US">and solid materials and left for degassing for 24 hours. </span><span lang="EN-US">The substrate in the AD process was a model mix</span><span lang="EN-US"> of FW.</span><span lang="EN-US">     </span><span lang="EN-US"> To ensure mix homogeneity; each food type was first manually shredded and dried at 105 °C. Next, the proper mass of each component was weighted and ground to 0.2-0.053 mm. After preparation, the material was dried again and secured in an air-tight vacuum-packed plastic bag. The proportion of individual food waste within the food waste mixture is depicted in Table 1. </span></span><span lang="EN-US" style="font-size:11pt"></span></p><p class="MsoNormal" style="margin:0in;color:rgb( 0 , 0 , 0 );letter-spacing:normal;font-size:12px"><span lang="PL" style="font-size:11pt"></span><span lang="EN-US" style="font-size:11pt">Table 1. Percentage, quantity, and features of food waste in the mix of used substrate. </span></p><p><img 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/><span lang="PL" style="font-size:11pt"></span><br /></p><p class="MsoNormal" style="margin:0in;font-size:12px"><span lang="PL" style="font-size:11pt"><span lang="EN-US">The anaerobic digestion process was performed using the automatic methane potential test system (AMPTS II, BPC Instruments, Sweden). The system consisted of 15 batch reactors placed in a water bath. Each reactor had a volume of 600 mL and was equipped with agitation. The reactors were kept in a water bath at a temperature of 37°C, with automatic stirrers agitating the solution for 2 minutes every hour.</span></span><strong><span lang="EN-US" style="font-size:11pt"></span></strong></p><p class="MsoNormal" style="margin:0in;color:rgb( 0 , 0 , 0 );letter-spacing:normal;font-size:12px"><span lang="PL" style="font-size:11pt"><span lang="EN-US">     </span><span lang="EN-US">To check the influence of different CMs on bio</span><span lang="EN-US">methane</span> <span lang="EN-US">production</span><span lang="EN-US">,</span><span lang="EN-US"> from FW, </span><span lang="EN-US"> 5 variants </span><span lang="EN-US">were </span><span lang="EN-US">studied</span><span lang="EN-US">. The first variant was control</span><span lang="EN-US">, </span><span lang="EN-US">inoculum </span><span lang="EN-US">only. The second variant </span><span lang="EN-US">consists of </span><span lang="EN-US">inoculum </span><span lang="EN-US">and</span><span lang="EN-US"> FW. The next </span><span lang="EN-US">three</span><span lang="EN-US"> variants consist of inoculum, FW, and specific CMs. 400 g of inoculum was placed in each reactor. For variants with substrate and CMs, 4.79 g of dry FW and 2 g of CMs were placed. Each variant was performed in triplicate. The AD process was carried out at 37°C for 21 days. <span lang="PL"></span>After the process&#39;s end, the digestate sample was collected and analyzed for volatile fatty acid content (VFAs). VFAs are a group of one of the most crucial chemical compounds during methanogenesis. The elemental composition of the digestate used to determine the substrate dose and CMs was 3,56 %<sub>TS</sub>, 62,09 %<sub>VS</sub>. Based on this, the substrate-to-inoculum ratio (ISR) was established at 2, allowing for the determination of the CMs and FW doses. The biogas measurements were automatically recorded in the AMPTS system (AMPTS II, BPC Instruments, Sweden), and following the process, the biogas was released.</span></span><span lang="EN-US" style="font-size:11pt">                                                                                             </span></p><p class="MsoNormal" style="margin:0in;font-size:12px"><span lang="PL" style="font-size:11pt"><strong><span lang="EN-US">Materials Analysis</span></strong></span><span lang="EN-US" style="font-size:11pt"></span></p><p class="MsoNormal" style="margin:0in;font-size:12px"><span lang="PL" style="font-size:11pt"><span lang="EN-US">The wheat straw and CMs were analyzed for total solids (TS), volatile solids (VS), moisture content (MC), ash content (AC), high heating value (HHV), reaction (pH), specific surface area (SSA) functional groups (FTIR) and elemental composition (C, H, N, S, O). The FW mixture was analyzed for MC, TS, VS, and elemental composition (C, H, N, S, O). The anaerobic digestion process residues (digestate) were analyzed for VFA content determination.   </span></span><span lang="EN-US" style="font-size:11pt"></span></p><p class="MsoNormal" style="margin:0in;font-size:12px"><span lang="PL" style="font-size:11pt"><span lang="EN-US">The MC, TS, VS, and AC were determined using a muffle furnace (8.1/1100; SNOL, Utena, Lativa) and laboratory dryer Wamed KBC-100W</span><span lang="EN-US">, </span><span lang="EN-US">Warsaw, Poland)</span><span lang="EN-US"> following PN-EN ISO 18134-2:2017-0 and PN-EN 15169:2011 standards, respectively. The VM was determined using thermogravimetry (Czylok, RST 40 × 200/100, Jastrzębie-Zdrój, Poland) following (Torquato et al. 2016). Measurements were made in triplicate. </span></span><span lang="EN-US" style="font-size:11pt"></span></p><p class="MsoNormal" style="margin:0in;font-size:12px"><span lang="PL" style="font-size:11pt"><span lang="EN-US">The pH analysis was conducted by mixing every material with water in a ratio of 1 to 10 followed by shaking for 2 hours (Induchoodan et al. 2024). The samples were shaken using an orbital shaker (ELMI DOS-20L). The pH in the solution was measured using a pH meter (Elmetron CPC-411). Measurements were made in triplicate and averaged using the arithmetic mean.</span></span><span lang="EN-US" style="font-size:11pt"></span></p><p class="MsoNormal" style="margin:0in;font-size:12px"><span lang="PL" style="font-size:11pt"><span lang="EN-US">For SSA analysis, a sample of about 0.2 g was used. The analysis was carried out using a sorption analyzer (ASAP 2020, Micromeritics, Atlanta, USA), using the volumetric method. Before the measurements, the materials were pre-degassed in a vacuum at 300 °C for 6 h. Then, nitrogen sorption was measured at 77 K. Based on the obtained isotherms, the SSA was determined following Brunauer–Emmett–Teller (BET) theory. It should be noted that the degassing temperature of the sample, which exceeded the production temperature of both hydrochar and the pyrolysis product (both materials produced at a temperature of 240 °C), may have influenced their properties, such as specific surface area and the presence or absence of certain organic compounds.</span></span><span lang="EN-US" style="font-size:11pt"></span></p><p class="MsoNormal" style="margin:0in;font-size:12px"><span lang="PL" style="font-size:11pt"><span lang="EN-US">The functional groups were determined using reflection-Fourier transform infrared (FTIR). The measurements were made using a Nicolet iN10 integrated infrared microscope with a Nicolet iZ10 external FT-IR module (Thermo Fischer Scientific, Waltham, MA, USA). For each spectrum, 32 scans were averaged in the mid-IR range of 400–4000 cm<sup>−1</sup>.</span></span><span lang="EN-US" style="font-size:11pt"></span></p><p class="MsoNormal" style="margin:0in;font-size:12px"><span lang="PL" style="font-size:11pt"><span lang="EN-US">The elemental composition was determined using an elemental analyzer (Perkin Elmer, 2400 Series, Waltham, MA, USA) following PN-EN ISO 16948:2015–07 standard</span></span><span lang="EN-US" style="font-size:11pt"></span></p><p><span style="font-size:12px"><br /></span></p><p class="MsoNormal" style="margin:0in;color:rgb( 0 , 0 , 0 );letter-spacing:normal;font-size:12px"><span lang="PL" style="font-size:11pt"><span lang="EN-US">For VFA analysis,</span></span><span lang="EN-US" style="font-size:11pt"> the samples underwent centrifugation at 10 °C at 4500 rpm for 10 minutes. Following this, they were diluted with Milli-Q water and recentrifuged at the same temperature for 5 minutes at 15000 rpm. Both quantitative and qualitative analyses were conducted using Ultra-High-Performance Liquid Chromatography (U-HPLC) with the UltiMate 3000 System from ThermoFisher Scientific, UK. A standard solution of VFA (Volatile Free Acid Mix, CRM46975, Merck, Poland) was prepared at a final concentration of 10 mM and stored at 4 °C following the manufacturer&#39;s instructions. The standard curve was established by appropriately diluting the analytes in Milli-Q water. Ethanol standards were also obtained from a supplier. The concentration of VFA and other components, including ethanol, was analyzed using a HyperREZ XPCarbohydrateH&#43; 8 </span><span lang="PL" style="font-size:11pt">μ</span><span lang="EN-US" style="font-size:11pt">m column (Thermo Scientific, Waltham, MA). Analyte identification was performed using a UV/VIS-DAD detector set at 208 ± 1 nm. A refractive index (RI) detector (Shodex, Ogimachi, Japan) was utilized concurrently to detect the potential presence of ethanol in the samples. The eluent used was 0.25 mM trifluoroacetic acid, with a flow rate of 1.1 mL/min under isocratic elution conditions, and the column temperature was maintained at 35 °C. Data was analyzed using Chromeleon 7.1 Software, with all samples analyzed in triplicate.</span></p>