Impacto de herbicidas em isolados de Trichoderma spp.

O uso de microrganismos é uma alternativa para o controle de doenças em plantas. Todavia, é prudente verificar a interação desse com os demais métodos de controle empregados em determinada cultura. Dessa forma, objetivou-se avaliar a fungitoxicidade dos herbicidas sobre o crescimento e desenvolvimento dos isolados de Trichoderma spp. Utilizou-se o delineamento inteiramente casualizado, em esquema fatorial 6 x 6 x 4, com quatro repetições. O fator A correspondeu aos herbicidas pendimethalin, clomazone, carfentrazone-ethyl, oxadiazon, thiobencarb + propanil e byspiribac-sodium; o fator B, às doses dos herbicidas - 0, 25, 50, 75, 100 e 200% da dose recomendada; e o fator C, aos isolados de Trichoderma spp. AJAM 18, CE 66, TRI 01 e TRI 02. O ensaio foi realizado em condições in vitro; avaliaram-se o crescimento micelial radial (CMR) e a esporulação dos isolados após aplicação dos herbicidas. Observaram-se diferenças de sensibilidade dos isolados para o mesmo produto testado. O oxadiazon reduziu o CMR dos isolados AJAM 18 e TRI 01 em 66 e 35%, respectivamente. No entanto, reduziu apenas 16% do CMR do isolado TRI 02 e não alterou o CMR do isolado CE 66 mesmo em 200% da dose recomendada. Verificaram-se diferentes efeitos dos produtos em cada isolado. A mistura comercial de thiobencarb+propanil foi altamente tóxica aos isolados de Trichoderma spp., com reduções em torno de 85% no CMR e no número de esporos. Por outro lado, o byspiribac-sodium pouco afetou os isolados, apresentando reduções inferiores a 10% no CMR e na esporulação. O carfentrazone-ethyl e byspiribac-sodium demonstraram ser compatíveis com os isolados de Trichoderma spp. estudados.

Manejo de Conyza bonariensis resistente ao glyphosate: coberturas de inverno e herbicidas em pré-semeadura da soja

Conyza bonariensis tornou-se a principal planta daninha da cultura da soja no Sul do Brasil, em decorrência da evolução para resistência ao herbicida glyphosate. O objetivo deste trabalho foi avaliar o efeito de diferentes coberturas de inverno e da associação de manejo de dessecação pré-semeadura da soja, visando ao controle de C. bonariensis resistente ao glyphosate. Um experimento foi conduzido em campo, na safra 2010/2011. Os tratamentos foram conduzidos em esquema de parcelas subdivididas, em que as coberturas de inverno foram alocadas nas parcelas principais: aveia-preta, nabo, ervilhaca, azevém, trigo e pousio. Nas subparcelas, foram alocados os tratamentos de manejo de dessecação pré-semeadura da soja: glyphosate (720 g e.a ha-1), glyphosate (720 g e.a ha-1) + 2,4-D (1.050 g e.a ha-1), glyphosate (720 g e.a ha-1) + 2,4-D (1.050 g e.a ha-1)/paraquat (200 g i.a ha-1) + diuron (100 g i.a ha-1), glyphosate (720 g e.a ha-1) + chlorimuron-ethyl (80 g i.a ha-1), glyphosate (720 g e.a ha-1) + chlorimuron-ethyl (80 g i.a ha-1)/paraquat (200 g i.a ha-1) + diuron (100 g i.a ha‑1) e roçada. O nabo foi a espécie de cobertura que produziu o maior volume de massa seca durante o inverno, enquanto a ervilhaca foi a que apresentou maior efeito supressor sobre a germinação e o desenvolvimento inicial de C. bonariensis. Associações de glyphosate com 2,4-D ou chlorimuron-ethyl, seguidas da aplicação sequencial de paraquat + diuron, causaram maior redução na infestação de C. bonariensis.

On-line determination of residual collector concentration in flotation process

Valuable minerals can be recovered by using froth flotation. This is a widely used separation technique in mineral processing. In a flotation cell hydrophobic particles attach on air bubbles dispersed in the slurry and rise on the top of the cell. Valuable particles are made hydrophobic by adding collector chemicals in the slurry. With the help of a frother reagent a stable froth forms on the top of the cell and the froth with valuable minerals, i.e. the concentrate, can be removed for further processing. Normally the collector is dosed on the basis of the feed rate of the flotation circuit and the head grade of the valuable metal. However, also the mineral composition of the ore affects the consumption of the collector, i.e. how much is adsorbed on the mineral surfaces. Therefore it is worth monitoring the residual collector concentration in the flotation tailings. Excess usage of collector causes unnecessary costs and may even disturb the process. In the literature part of the Master’s thesis the basics of flotation process and collector chemicals are introduced. Capillary electrophoresis (CE), an analytical technique suitable for detecting collector chemicals, is also reviewed. In the experimental part of the thesis the development of an on-line CE method for monitoring the concentration of collector chemicals in a flotation process and the results of a measurement campaign are presented. It was possible to determine the quality and quantity of collector chemicals in nickel flotation tailings at a concentrator plant with the developed on-line CE method. Sodium ethyl xanthate and sodium isopropyl xanthate residuals were found in the tailings and slight correlation between the measured concentrations and the dosage amounts could be seen.

Rapid diagnosis of resistance to imidazolinone herbicides in barnyardgrass (Echinochloa crus-galli) and control of resistant biotypes with alternative herbicides

The resistance of barnyardgrass (Echinochloa crus-galli) to imidazolinone herbicides is a worldwide problem in paddy fields. A rapid diagnosis is required for the selection of adequate prevention and control practices. The objectives of this study were to develop expedite bioassays to identify the resistance to imidazolinone herbicides in barnyardgrass and to evaluate the efficacy of alternative herbicides for the post-emergence control of resistant biotypes. Three experiments were conducted to develop methods for diagnosis of resistance to imazethapyr and imazapyr + imazapic in barnyardgrass at the seed, seedling and tiller stages, and to carry out a pot experiment to determine the efficacy of six herbicides applied at post-emergence in 13 biotypes of barnyardgrass resistant to imidazolinones. The seed soaking bioassay was not able to differentiate the resistant and susceptible biotypes. The resistance of barnyardgrass to imidazolinones was effectively discriminated in the seedlings and tiller bioassays seven days after incubation at the concentrations of 0.001 and 0.0001 mM, respectively, for both imazethapyr and imazapyr + imazapic. The biotypes identified as resistant to imidazolinones showed different patterns of susceptibility to penoxsulam, bispyribac-sodium and pyrazosulfuron-ethyl, and were all controlled with profoxydim and cyhalofop-butyl. The seedling and tiller bioassays are effective in the diagnosis of barnyardgrass resistance to imidazolinone herbicides, providing an on-season opportunity to identify the need to use alternative herbicides to be applied at post-emergence for the control of the resistant biotypes.

Effect of plant regulators on growth and flowering of 'Meyer' zoysiagrass

This trial aimed to evaluate the effect of sequential applications of different plant regulators over growth and flower rachis emission of 'Meyer' zoysiagrass (Zoysia japonica). The study was conducted on 15-month old green turfgrass under a randomized complete block design with four replications. The following plant regulator and doses were tested: trinexapac-ethyl (113+113, 226+113, 226+226, 452+113, 452+226, 452+452, 678+339 e 904+452 g a.i./ha-1), prohexadione-calcium (100+100 e 200+200 g a.i. ha-1) and bispyribac-sodium (40+40 e 60+60 g a.i. ha-1), as well as an untreated control. The turfgrass was mowed again at 3.0 cm aboveground and the second plant regulator was applied when 'Meyer' zoysiagrass was between 5.0 and 6.0 cm high. The effect of the treatments was visually rated for visual injury, plant height, height and number of flower rachis, and total dry mass production of clippings. Only bispyribac-sodium had visual symptoms of injury on 'Meyer' zoysiagrass, and no intoxication was observed at 28 days after the second application (DAAB). The sequential applications of trinexapac-ethyl, prohexadione-calcium and bispyribac-sodium reduced by more than 80% the total clipping dry mass produced by 'Meyer' zoysiagrass. All the plant regulators tested also showed promising results in reducing the height and emission of rachis, especially when trinexapac-ethyl was applied at the doses 452+452, 678+339 and 904+452 g a.i. ha-1. 'Meyer' zoysiagrass turfgrass can be handled with the sequential application of a plant regulator, which reduces the need for mowing over a period up to 110 days after the application of the second plant regulator, and it also avoids deleterious visual effects over turfgrass.

Globe fringerush (Fimbristylis miliacea) cross resistance to als-inhibitor herbicides under field conditions in irrigated rice in the south of Brazil

ALS-inhibiting herbicides usually provide adequate weed control in irrigated rice fields. After consecutive years of use, the Cyperaceae species, globe fringerush (Fimbristylis miliacea) began to show resistance to ALS (acetolactate synthase) inhibitors. Globe fringerush is one of the most problematic herbicide-resistant weeds in irrigated rice in the state of Santa Catarina in the South of Brazil. The objective of this research was to examine cross resistance of globe fringerush to ALS inhibitors, under field conditions. Two experiments were conducted in a rice field naturally infested with ALS-resistant globe fringerush in Santa Catarina, in the 2008/09 and 2009/10 cropping seasons. The experimental units were arranged in randomized complete block design, with five replicates, consisting of two factors (herbicide and dose) in a 4 x 5 factorial arrangement. ALS herbicides included bispyribac-sodium, ethoxysulfuron, pyrazosulfuron-ethyl and penoxsulam. Six-leaf globe fringerush was sprayed with herbicide doses of 0, 0.5, 1, 2 and 4X the recommended doses in a spray volume of 200 L ha-1. The number of rice culm, filled and sterile grains, plant height, dry shoot biomass and grain yield were recorded. Globe fringerush control was evaluated 28 and 70 days after herbicide application (DAA); shoots were harvested at 13 weeks after herbicide application and dry weight recorded. Competition with globe fringerush reduced the number of culm and rice grain yield. The globe fringerush biotype in this field was resistant to all ALS herbicides tested. Penoxsulam had the highest level of activity among treatments at 28 and 70 DAA, but the control level was only 50% and 42%, respectively, in the second year of assessment. This was not enough to prevent rice yield loss. Alternative herbicides and weed control strategies are necessary to avoid yield losses in rice fields infested with ALS-resistant biotypes of globe fringerush.

Herbicide selectivity in alfalfa crops

This study aimed to determine the selectivity of herbicides applied in pre- and post-emergence for alfalfa crops. Three separate experiments were carried out under greenhouse conditions. The first experiment was arranged in a completely randomized design with three replications in a 4 x 11 + 1 factorial scheme , with eleven herbicides (bentazon, chlorimuron-ethyl, fomesafen, fluazifop-p-butyl, saflufenacil, imazethapyr, clethodim, nicosulfuron, imazaquin, haloxyfop-methyl and MSMA), four doses of each herbicide (0.5 D, 0.75 D, 1.0 D and 1.25 D, where D = recommended dose), plus an untreated control. The products were applied to alfalfa plants at the stage of 4 to 5 leaf pairs. In the second experiment, the effect of pre-emergent herbicides on early alfalfa development was observed through a completely randomized design with five replications in a 3 x 4 x 2 factorial scheme, with three herbicides (hexazinone, atrazine + simazine, S-metolachlor), four doses (0.5 D, 0.75 D, 1.0 D and 1.25 D), and two types of soil texture (loamy and clay soil), plus an untreated control. The third experiment evaluated the action of atrazine, 2,550 g ha-1; clomazone - 600 g ha-1; diclosulam - 25 g ha-1; diuron+hexazinone - 936 + 264 g ha-1 and diuron+hexazinone +sulfometuron - 1,386 + 391 + 33.35 g ha-1 on alfalfa sown at different times after herbicide application. The effects of the treatments on alfalfa were evaluated according to visual phytotoxicity symptoms, plant height, and biomass of roots and shoots. Among the herbicides applied at post-emergence, imazethapyr, clethodim, haloxyfop-p-methyl and MSMA were selective for alfalfa, while among those applied at pre-emergence, none were selective, regardless of soil texture. The results of the third experiment showed that the herbicides diclosulam, hexazinone + diuron and atrazine caused less toxicity in alfalfa plants.

Effect of selectivity of herbicides and plant growth regulators used in sugarcane crops on immature stages of Trichogramma galloi (Hymenoptera: Trichogrammatidae)

Herbicides and plant growth regulators are often used in sugarcane management. However, the use of non-selective pesticides can cause adverse effects on the efficiency of beneficial insects in integrated pest management. Within this context, this study aimed to evaluate the effect of such products on the immature stages of the parasitoid Trichogramma galloi. Eggs of Diatraea saccharalis containing the parasitoid at the egg-larva stage and at the prepupal and pupal stages were immersed in test solutions of the following pesticides (maximum recommended doses for sugarcane): herbicides clomazone and diuron + hexazinone, and plant growth regulators trinexapac-ethyl and sulfometuron-methyl. The biological properties evaluated were emergence (F1 and F2) and number of eggs parasitized by T. galloi (F1). The products were classified according to percentage of reduction in emergence and parasitism: harmless (<30%), slightly harmful (30-79%), moderately harmful (80-99%) and harmful (>99%). The pesticides evaluated were considered to be harmless or slightly harmful to immature T. galloi and, thus, their use should be preferred for preserving this parasitoid species in sugarcane management programs.

Multiple resistance of Conyza sumatrensis to Chlorimuron­ethyl and to Glyphosate

Weed resistance to herbicides has been a major issue in Brazil, mainly due to the inefficiency of the herbicides used in no-till areas and to the high cost of these herbicide treatments. Failures in controlling the weed Conyza have been reported in Western and Northern grain crop areas in Paraná (Brazil). This work aimed to evaluate the potential occurrence of C. sumatrensis biotypes resistant to the herbicides chlorimuron-ethyl and glyphosate. Experiments were carried out under greenhouse conditions with four biotypes (Cascavel-2, Toledo-4, Tupãssi-6, and Assis Chateaubriand-7) possibly resistant to, as well as a population considered susceptible to chlorimuron-ethyl and glyphosate. To obtain dose-response curves, eight herbicide doses of chlorimuron-ethyl (0, 2.5, 5, 10, 20, 40, 80 and 160 g ha-1) and glyphosate (0, 90, 180, 360, 720, 1,440, 2,880 and 5,760 g e.a. ha-1) were applied and weed control and shoot biomass evaluations were made. Results provided evidence that two biotypes (Cascavel-2 and Tupãssi-6) were resistant to glyphosate and four biotypes (Cascavel-2, Toledo-4, Tupãssi-6 and Assis Chateaubriand-7) were resistant to chlorimuron­ethyl. Multiple resistance to glyphosate and chlorimuron was confirmed for biotypes Cascavel­2 and Tupãssi 6. This is the first report on multiple resistance in Conyza sumatrensis, worldwide.

PHYSIOLOGICAL QUALITY OF SOYBEAN SEEDS DEPENDING ON THE PREHARVEST DESICCATION

ABSTRACTDepending on the cultivar, the use of desiccants in the preharvest can favor maintenance of physiological quality. The objective of the study was to assess the physiological quality of soybean seeds as due to the use of apreharvest desiccant and desiccation time in two harvests (2011/12 and 2012/13). The treatments were five soybean cultivars, two growth stages of application, a control (without desiccant application), and three desiccants (glufosinate-ammonium, carfentrazone-ethyl and paraquat) (2011/12 harvest). In the 2012/13 harvest the carfentrazone-ethyl desiccant was replaced by diquat. The physiological quality of seeds was assessed by the percentage of viability and vigor (cold test, tetrazolium test and accelerated aging test). In 2011/12 harvest, there was an early harvest in six days with the use of glufosinate-ammonium and paraquat desiccants, when desiccation was done in stage R7.1, with maintenance of seed quality; however it was dependent on the cultivar. In the 2012/13 harvest there was no early harvesting due to the presence of rain in the preharvest and the use of desiccation did not affect the physiological quality of the seeds either. Cultivar NA5909 RG was more tolerant to remaining in the cultivation environment and maintained higher viability than 90% and greater vigor of 71% by the cold test compared to cultivar BMX Turbo (2011/12 harvest). It is concluded that desiccation can be a viable alternative to the soybean early harvesting, but it depends on the cultivar, the time of desiccation, the active principle of the desiccant and the absence of rain in preharvest.

SELECTION OF HERBICIDES TARGETING THE USE IN CROP SYSTEMS CULTIVATED WITH SHOWY CROTALARIA

ABSTRACT The increase in the area planted with Crotalaria spectabilishas occurred by several factors, highlighting the potential to reduce the nematodes, nitrogen fixation and the high production of biomass. By becoming a species sown as a crop, it is necessary to control the weeds that coexist with showy crotalaria. This change in the use of this crop creates the possibility of this specie becoming a weed. The aim of this study was to assess the potential use of herbicides applied in preemergence and postemergence of C.spectabilisfor different purposes (control of volunteer and selectivity plants). Three experiments were installed in a greenhouse (two with herbicides applied in preemergence - in soils with distinct textural categories; and one experiment with herbicides applied in postemergence). The results of the experiments with herbicides applied in preemergence showed that: amicarbazone, atrazine, diuron, metribuzin, prometryn, fomesafen and sulfentrazone showed effectiveness for control of C.spectabilis in clayey soil. Besides these, flumioxazin and isoxaflutole also showed potential to be used in the control of showy crotalaria in soils with loam texture. In relation to the postemergence herbicides, atrazine, diuron, prometryn, flumioxazin, fomesafen, lactofen, saflufenacil, amonio-glufosinate and glyphosate can be used aiming the chemical control of C.spectabilis. Herbicides chlorimuron-ethyl, diclosulan, imazethapyr, pyrithiobac-sodium, trifloxysulfuron-sodium, clomazone, pendimethalin, S-metolachlor and trifluralin applied in preemergence, and imazethapyr, pyrithiobac-sodium, flumiclorac, bentazon and clethodim applied in postemergence caused low levels of injury to C.spectabilis plants, making necessary the development of new searches to ensure the selectivity of these products.

WEED MANAGEMENT WITH HERBICIDES APPLIED IN PRE AND POSTEMERGENCE ON CASTOR CROP

ABSTRACT The aim of this work was to evaluate the weed management with herbicides applied in pre and postemergence on castor crop. The treatments were constituted by management systems using herbicides in pre (PRE) and postemergence (POS): 1) S-metolachlor at 576 g ha-1 (PRE 1) and chlorimuron-methyl at 15 g ha-1 (POS 1); 2) PRE 1 + clomazone at 650 g ha-1(PRE 2) and POS 1; 3) PRE 1, POS 1 and halosulfuron-methyl at 112.5 g ha-1(POS 2); 4) PRE 1, POS 1 and ethoxysulfuron at 60 g ha-1 (POS 3); 5) PRE 1, POS 1 and ethoxysulfuron at 120 g ha-1 (POS 4); 6) PRE 1 + PRE 2, POS 1 and POS 2; 7) PRE 1 + PRE 2, POS 1 and POS 3; 8) PRE 1 + PRE 2, POS 1 and POS 4; 9) hand-hoeing control and 10) non-weeded control. The experimental design was randomized blocks with four replications. The association of the herbicides in PRE combined to sequence applications of chlorimuron-ethyl and halosulfuron-methyl or ethoxysulfuron in POS resulted in the highest control levels of Richardia scabraand Cyperus ferax. Mild phytointoxication symptoms to the crop were more persistent with ethoxysulfuron at 120 g ha-1. The acceptable control of the weed species and similar yield to the hand-hoeing control permitted to conclude that S-metolachlor + clomazone PRE, followed by chlorimuron-ethyl and halosulfuron-methyl POS proved to be more adequate as a weed management strategy on castor crop.

CHEMICAL CONTROL OF WHITE CLOVER IN SOYBEAN CROPS

ABSTRACTWhite clover is tolerant to many herbicides, making difficult a chemical control of this species during soybean crop establishments. The objective of this research was to select herbicides applied postemergence to control white clover in soybean and know the effects of this control on soybean yield. Seven herbicides were assessed, applied postemergence, with or without sequential application of glyphosate, and two control treatments (no control and total control of white clover). Glyphosate (with two sequential applications), fomesafen (with a sequential application of glyphosate), chlorimuron-ethyl and lactofen have shown a satisfactory control of white clover (above 80%). The lower control efficiency has resulted in lower production of soybeans.

REGULADOR DE CRESCIMENTO NA PRODUTIVIDADE E QUALIDADE DE SEMENTES DE AVEIA-BRANCA

RESUMO A aveia-branca (Avena sativa) é uma importante alternativa para cultivos de inverno no sul do Brasil. Contudo, elevados percentuais de acamamento limitam sua produtividade. Nesse contexto, a utilização de reguladores de crescimento pode ser uma opção para evitar o acamamento e obter maior produtividade. O objetivo deste trabalho foi avaliar o efeito de doses do regulador de crescimento trinexapac-ethyl sobre as características agronômicas da aveia-branca, bem como sua influência na qualidade fisiológica e sanitária das sementes. Um experimento foi conduzido em campo, onde foi avaliada a influência de quatro doses de trinexapac-ethyl (0, 50, 100 e 150 g i.a. ha-1) sobre a estatura de planta, o diâmetro de colmo, o percentual de acamamento e os componentes do rendimento. Um segundo experimento foi conduzido em laboratório, onde sementes provenientes do estudo em campo foram avaliadas quanto a qualidade fisiológica a partir da mensuração da germinação, primeira contagem da germinação, condutividade elétrica, comprimento e massa de plântulas, envelhecimento acelerado, teste de frio, índice de velocidade de germinação, índice de velocidade de emergência, massa seca de plântulas em campo e sanidade pelo método de Blotter Test. A utilização de doses crescentes de trinexapac-ethyl reduziu de forma quadrática a estatura, bem como o acamamento de plantas de aveia-branca. A dose de 100 g i.a ha-1 de regulador de crescimento proporcionou os melhores resultados para os componentes de produtividade em A. sativa. O uso do trinexapac-ethyl afeta negativamente a germinação e o vigor de sementes de aveiabranca, assim como a sua sanidade, reduzindo a capacidade de estabelecimento e desenvolvimento inicial da cultura.

Ionic liquid mediated biomass deconstruction: from analysis challenges to fermentable sugars

Ionic liquids, ILs, have recently been studied with accelerating interest to be used for a deconstruction/fractionation, dissolution or pretreatment processing method of lignocellulosic biomass. ILs are usually utilized combined with heat. Regarding lignocellulosic recalcitrance toward fractionation and IL utilization, most of the studies concern IL utilization in the biomass fermentation process prior to the enzymatic hydrolysis step. It has been demonstrated that IL-pretreatment gives more efficient hydrolysis of the biomass polysaccharides than enzymatic hydrolysis alone. Both cellulose (especially cellulose) and lignin are very resistant towards fractionation and even dissolution methods. As an example, it can be mentioned that softwood, hardwood and grass-type plant species have different types of lignin structures leading to the fact that softwood lignin (guaiacyl lignin dominates) is the most difficult to solubilize or chemically disrupt. In addition to the known conventional biomass processing methods, several ILs have also been found to efficiently dissolve either cellulose and/or wood samples – different ILs are suitable for different purposes. An IL treatment of wood usually results in non-fibrous pulp, where lignin is not efficiently separated and wood components are selectively precipitated, as cellulose is not soluble or degradable in ionic liquids under mild conditions. Nevertheless, new ILs capable of rather good fractionation performance have recently emerged. The capability of the IL to dissolve or deconstruct wood or cellulose depends on several factors, (e.g. sample origin, the particle size of the biomass, mechanical treatments as pulverization, initial biomassto-IL ratio, water content of the biomass, possible impurities of IL, reaction conditions, temperature etc). The aim of this study was to obtain (fermentable) saccharides and other valuable chemicals from wood by a combined heat and IL-treatment. Thermal treatments alone contribute to the degradation of polysaccharides (e.g. 150 °C alone is said to cause the degradation of polysaccharides), thus temperatures below that should be used, if the research interest lies on the IL effectiveness. On the other hand, the efficiency of the IL-treatment can also be enhanced to combine other treatment methods, (e.g. microwave heating). The samples of spruce, pine and birch sawdust were treated with either 1-Ethyl-3-methylimidazolium chloride, Emim Cl, or 1-Ethyl-3-methylimidazolium acetate, Emim Ac, (or with ionized water for comparison) at various temperatures (where focus was between 80 and 120 °C). The samples were withdrawn at fixed time intervals (the main interest treatment time area lied between 0 and 100 hours). Double experiments were executed. The selected mono- and disaccharides, as well as their known degradation products, 5-hydroxymethylfurfural, 5-HMF, and furfural were analyzed with capillary electrophoresis, CE, and high-performance liquid chromatography, HPLC. Initially, even GC and GC-MS were utilized. Galactose, glucose, mannose and xylose were the main monosaccharides that were present in the wood samples exposed to ILs at elevated temperatures; in addition, furfural and 5-HMF were detected; moreover, the quantitative amount of the two latter ones were naturally increasing in line with the heating time or the IL:wood ratio.