Respuestas, 24 (2), May - August 2019,, pp. 27-38, ISSN 0122-820X - E ISSN: 2422-5053

Journal of Engineering Sciences

rigin rie https://doi.org/10.22463/0122820X.1828 Chemical and thermal characterization of the construction material of of seven species of from Norte de Santander - Colombia. Caracterización química y térmica del material de construcción de nidos de siete especies de avispas del Norte de Santander - Colombia. María Del Carmen Parra Hernández1, Diana Alexandra Torres Sánchez2* 1Chemistry, [email protected], orcid.org/0000-0003-2034-4495, Universidad de Pamplona, Pamplona, Colombia 2*PhD in Chemistry Sciences, [email protected], orcid.org/0000-0002-0602-9299, Universidad de Pamplona, Pamplona, Colombia.

How to cite: M.C. Parra-Hernadez y D.A. Torres-Sanchez , “Chemical and thermal characterization of the construction material of nests of seven species of wasps from Norte de Santander - Colombia.”. Respuestas, vol. 24, no. 2, pp. 27-38, 2019.

Received on August 09, 2018; Approved on November 10, 2018

ABSTRACT Social wasps are that construct their nests using pulp, plant and themselves secretions for Keywords: the accomplishment of their activities as a colony. Currently in Colombia, there is little knowledge about this interesting material due to its characteristics, which could be used in promising applications. In this Wasps, work the chemical and thermal characterization of nests of seven species of wasps ( pallipes, Nests, , Agelaia areata, Polybia aequatorialis, Parachartergus apicalis, Mischucytharus imitator, Thermogravimetric lecheguana) living in Norte de Santander, was carried out with the purpose of establishing if there are significant differences between species and provide information that could be used as a model or Analysis (TGA), precursors for the synthesis in biomimetics and / or nanotechnology. Thermogravimetric analysis (TGA) Differential Scanning and differential scanning calorimetry (DSC) were performed using a Thermal analyser SDT-Q600 from T.A. Calorimetry (DSC), Instruments. An infrared spectrophotometer FT-IR SHIMADZU Prestige-21 with ATR was used for infrared Fourier Transform Infrared analysis. The fluorescence analysis (XRF) was performed using a sequential X-ray fluorescence spectrometer Spectroscopy (FTIR), of dispersive wavelength of 4kW BRUKER model S8 TIGER. The thermogravimetric analysis shows three mass losses and four degradation processes related to moisture loss, degradation of hemicellulose, X-ray Fluorescence (XRF). cellulose and lignin. The infrared analysis allowed identifying characteristic functional groups of cellulose, hemicellulose and lignin. Through the X-ray fluorescence analysis, some metals such as K, Ca, Al, Mg, Ti, Cr, Mn, Fe, Ni, Cu, Zn, Se and Li were found. The analyses made of the samples allowed to establish differences and similarities in the construction material of the studied species.

RESUMEN Las avispas sociales son insectos que construyen sus nidos utilizando pulpa de madera, secreciones de Palabras clave: plantas y de diferentes partes de su cuerpo que requieren para la realización y ejecución de sus actividades como colonia. Actualmente en Colombia se tiene poco conocimiento acerca de este material que podría Avispas, aprovecharse en diferentes aplicaciones. En el presente trabajo se realizó la caracterización química y Nidos, térmica de nidos de siete especies de avispas (, Agelaia multipicta, Agelaia areata, Polybia aequatorialis, Parachartergus apicalis, Mischucytharus imitator, ) de Norte de Análisis Santander con motivos de establecer si existen diferencias significativas entre especies y proporcionar Termogravimétrico (TGA), información que sea la base de otras investigaciones encaminadas hacia la utilización de estos materiales Calorimetría Diferencial como modelos o precursores de síntesis en biomimética y/o nanotecnología. Los análisis termogravimétrico (TGA) y calorimetría diferencial de barrido (DSC) se realizaron empleando un equipo SDT-Q600 de de barrido (DSC), T.A. Instruments. Para el análisis infrarrojo se utilizó un espectrofotómetro infrarrojo FT-IR SHIMADZU Espectrofotometría Prestige-21 con ATR. El análisis de fluorescencia (XRF) se realizó empleando un espectrómetro secuencial Infrarroja (FTIR), de fluorescencia de rayos X de longitud de onda dispersiva de 4kW marca BRUKER modelo S8 TIGER. Fluorescencia de Rayos x En el análisis termogravimétrico se encontraron tres pérdidas de masa y cuatro procesos de degradación relacionados con la pérdida de humedad, la degradación de hemicelulosa, celulosa y lignina. El análisis (XRF). infrarrojo permitió determinar grupos funcionales característicos de celulosa, hemicelulosa y lignina. A través del análisis de fluorescencia de rayos X, se detectaron los metales K, Ca, Al, Mg, Ti, Cr, Mn, Fe, Ni, Cu, Zn, Se y Li. Los análisis realizados permitieron establecer diferencias y similitudes en el material de construcción de las diferentes especies.

*Corresponding E-mail luis.dominguez@ (Luis Pérez Domínguez) Peer review is the responsibility of the Universidad Francisco de Paula Santander. This isPeer an article review under is the the responsibility license CC ofBY-ND the Universidad Francisco de Paula Santander. This is an article under the license CC BY-NC-ND Chemical and thermal characterization of the construction material of nests of seven species of wasps from Norte de Santander - Colombia.

Wasps are insects of the order of and forms and processes of nature, which can be copied to suborder apocrite [1],[2]. Hymenoptera are one of the sustainably and effectively improve the design of different richest metazoan orders on the planet with about 115,000 processes and services required by humans [15],[16]. In to 199,000 species described [3],[4],[5],[6]. Wasps are addition, bioengineering and biotechnology have taken important within tropical ecosystems because they are advantage of many biological models to understand and insects used in biogeographic and ecological studies, as solve problems that may be related to food production, potential biological control agents, in comprehensive pharmaceuticals, and the health of human beings and studies involving other zoological and floristic groups, [17]; in the field of health, in the creation of and as bioindicators of regional ecological conditions. nanoparticles for biomedical purposes [18].

Biologically, they are characterized by building This study was carried out for the purpose of chemically collective nests made of chewed wood pulp. The social and thermally characterizing the nests built by seven wasps are organized in three castes, the reproductive species of wasps from Norte de Santander, Colombia, females (queens) in charge of laying eggs, the sterile and to establish whether there are significant differences females (workers) and the males. Once they have built between species and to provide information to serve as their nests, by chewing wood fibers, they deposit their the basis for other research aimed at the use of these eggs in compartments or cells, where they develop into materials in different applications.. larvae and pupae, emerging as adults [7],[8]. In temperate regions, a colony lasts only one season: queens being Materials and methods paired hibernate for about 90 days to emerge in spring and form new colonies; workers live for short periods of Sampling time, while males generally die after fertilizing the queen [9]. samples of species were collected in According to nesting sites, ethno-species build their nests different municipalities of the department of Norte de on three types of substrates: constructions, terrestrial and Santander; Agelaia pallipes, Parachartergus apicalis and vegetal or arboreal. The first refers to sites and materials Mischucytharus imitator (Pamplonita), Agelaia multipicta of anthropogenic origin [10]. Terrestrial substrate refers (Carmen de Tonchala), Agelaia areata and Polybia to natural cavities or abandoned cavities, and plant aequatorialis (Cúcuta). Abandoned nests were collected substrate includes weeds, shrubs, leaves, tree branches and stored in airtight plastic bags during transport from and hollow trunks [11], the latter being used by most the collection site to the laboratory. ethno-species for the establishment of their colonies. In The identification of the wasp species was carried out by the nests, several central activities of the colony occur, an expert, who examined adult specimens by means of such as the reuse of breeding cells, care of immatures observations under the stereomicroscope at 10X and 30X until the emergence in adults, provision of chewed prey taking into account the morphological identification keys for their offspring, trophylaxis and reproductive time for them. division of labor [12],[13],[5]. Instruments, materials and reagents The way in which the nests are built and the characteristics of the material needed to do so highlight the interest of For the present study we used a SDT Q-600 thermal these social insects as models for different human needs, analyser from TA Instruments, an FT-IR SHIMADZU especially for bioclimatic architectural designs and the Prestige-21 infrared spectrometer with ATR and a 4kW design of new materials [14]. Currently, the air circulation dispersive wavelength X-ray fluorescence sequential system in wasp and termite nests is being applied in the spectrometer BRUKER model S8 TIGER. optimization of energy consumption in different human constructions [12]. Thermal analysis DSC - TGA

In recent years, biomimetics has been inspired by Thermoanalytic determinations were performed using biological designs, consisting of the imitation of TA Instruments’ SDT Q-600 thermal analyzer which

Respuestas, 24 (2), pp. 27-38 , 2019, ISSN 0122-820X - E ISSN: 2422-5053 28 María Del Carmen Parra Hernández, Diana Alexandra Torres Sánchez simultaneously performs thermogravimetric analysis light elements a flow detector, the X-ray source was a (TGA) and differential scanning calorimetry (DSC). Rhodium tube (Rh) and the high precision goniometer The analysis was performed using between 10-20 mg of used for theta and 2 theta angles. pulverized sample, and it was introduced in an alumina cell. The analysis parameters were: heating ramp of 10 Statistical analysis ºC/min, from ambient temperature ̴ 20 ºC to 700 ºC in nitrogen atmosphere with a flow of 100 mL/min. Thermal properties were determined using Universal Analysis 2000 software (T.A. Instruments, Delaware, Fourier transform infrared spectroscopy (FTIR) USA). The results of the thermal analysis were analyzed with the statistical package of the program Origin pro A SHIMADZU IR Prestige-2.1 infrared spectrophotometer evaluation version and the statistical software XLSTAT was used using the attenuated total reflection (ATR) for Microsoft Excel trial version. Variance analysis technique, the spectra were obtained in the mid-infrared (ANOVA) was used to find if there were significant region, at wavelengths of 600 to 4000 cm-1, with a total differences between the different values obtained. of 40 scans and a resolution of 4 cm-1. X-ray fluorescence (XRF) Results and analysis

The XRF analysis was performed using the QUANT- Thermogravimetry (TGA) EXPRESS method (fundamental parameters) in the By means of thermogravimetric analysis (TGA - DTG) sodium (Na) to uranium (U) range, in a 4kW dispersive four mass loss processes were determined in the samples wavelength X-ray fluorescence sequential spectrometer (Figure 1) of the different species. Table I presents the BRUKER model S8 TIGER. To detect the heavy results of the temperatures involved and the percentage elements a Scintillation detector was used and for thes. of mass loss in each one.multipicta with the samples of

According to Figure 1, initially there was a loss of mass Statistical analysis reveals that significant differences between 50.32 ± 0.84 °C and 87.45 ± 6.74 °C attributed occur between the nests of the species A. areata with to the loss of water in the form of moisture absorbed the nests of the species M. imitator, as well as for the at the surface of the nest, in addition to this there were samples of the species A. areata with the samples of P. three other processes of loss of mass. The first T1 at apicalis, the samples of B. lecheguana with the samples 200.39 ± 2.34 °C - 238.58 ± 1.80 °C attributed to the of M. imitator, the samples of P. aequatorialis with the of hemicelluloses [19]. samples M. imitator, A.

29 Respuestas, 24 (2), pp. 27-38, 2019, ISSN 0122-820X - E ISSN: 2422-5053 Chemical and thermal characterization of the construction material of nests of seven species of wasps from Norte de Santander - Colombia.

M. imitator corroborating in this way, that the differences this peak occurred in the nests of the species M. imitator found in the chemical profile of the nests of the different with 319.66 ± 2.01 °C, P. apicalis with 322.22 ± 0.34 °C species is directly related to the chewing process of the and A. multipicta with 323.80 ± 7.45 °C, the samples that vegetable material used and the mixture that the wasps registered the highest value were the nests of A. pallipes add through oral secretions when building the nests [20] with 350.95 ± 8.15 °C and B. lecheguana with 345.83 ± . Studies such as that of M.R. Cole [21], in the nests 0.54 °C. Likewise, the analysis of variance reveals that the of three species of social wasps (), affirm that samples that present significant differences are: the nest the choice of type of plant material, plant fibers and the samples of the species A. pallipes with the nest samples duration of chewing of the materials affects the physical of the species P. apicalis, samples that were collected in and chemical characteristics of the construction material the municipality of Pamplona. There are also differences of the nest. Kazuyiki Kudo [22], in his study states between A. pallipes with A. multipicta and B. lecheguana that oral secretions physically protect the nest from the with P. apicalis. elements and the processing of the pulp is an aspect that could affect the absorption capacity of the nest paper and According to the degradation temperatures recorded in its durability. Also, the study by Khalid Khan [23], found the nest samples, the samples with the lowest value of that the architectural pattern of the nest and the chemical T1 (°C) were the species M. imitator, P. apicalis and composition vary among different species depending A. multipicta. This could be associated with increased on aspects such as salivary secretions that these insects volatility of the extractive (low molecular weight add to the material, environmental factors and material compounds) and hemicelluloses in the material, which selection. probably results in reduced temperatures corresponding to the degradation of components such as hemicellulose On the other hand, studies such as that of W.J. Etges [24], and lignin, because degradation of one component in the agree that although the place of nesting can influence the material may accelerate the degradation of the others composition and thermal behaviour of the nest material, [19]. Likewise, the low degradation temperature in the other aspects such as the environment in which wasp nests of M. imitator, P. apicalis and A. multipicta can lead colonies carry out nesting and other factors not only to undesirable properties such as browning and decreased genetic, but also exogenous (climate, rain, heat, cold, mechanical resistance when subjected to temperatures humidity, among others) must be considered. above 200°C. The degradation of one component in the material can accelerate the degradation of the others [19], and the low degradation temperature in the nests The second process, whose mass loss temperature T2 of M. imitator, P. apicalis and A. multipicta can lead to (°C) occurs from 287.44 ± 2.87 °C to 309.99 ± 1.23 °C undesirable properties such as browning and decreased corresponds to the shoulder present in the DTG curve and mechanical resistance when subjected to temperatures is associated with cellulose decomposition; the lowest above 200°C. values were identified in the M species samples. imitator with 287.44 ± 2.87°C, A. multipicta with 297.24 ± 4.65°C and P. apicalis with 298.79 ± 3.59°C, the samples of the species recording the highest temperature for this peak were A. areata with 309.39 ± 1.23°C, B. lecheguana with 307.10 ± 4.65°C and A. pallipes with 306.02 ± 8.12°C. The samples of the species recording the highest temperature for this peak were A. areata with 309.39 ± 1.23°C, B. lecheguana with 307.10 ± 4.65°C and A. pallipes with 306.02 ± 8.12°C. For this loss of mass there were no statistically significant differences between the nest samples according to the Bonferroni test. The third process related to temperature T3 (°C), occurs from 319.66 ± 2.01 °C to 350.95 ± 8.15 °C, corresponds to the decomposition of lignin. The lowest temperature for

Respuestas, 24 (2), pp. 27-38 , 2019, ISSN 0122-820X - E ISSN: 2422-5053 30 María Del Carmen Parra Hernández, Diana Alexandra Torres Sánchez

TGA and DTG curves for the nests of the wasp species studied. A) A. pallipes, B) A. multipicta, C) A. areata, D) P. aequatoria- lis, E) P. apicalis, F) M. imitator, G) B. lecheguana

31 Respuestas, 24 (2), pp. 27-38, 2019, ISSN 0122-820X - E ISSN: 2422-5053 Chemical and thermal characterization of the construction material of nests of seven species of wasps from Norte de Santander - Colombia.

Differential scanning calorimetry (DSC) endothermic in a range between 309.98 ± 1.54°C - 358.63 ± 2.34°C, related to the cellulose fraction, for this transition Table II shows the results obtained by differential scanning is included the enthalpy related to the degradation of the calorimetry. The corresponding thermographs are crystalline part of the cellulose for the nests of the species presented in Figure 2. The thermographs show between studied. Finally, there are two exothermic transitions, one 4 and 5 transitions. The first transition corresponds to a of them between 393.63 ± 2.65°C - 451.21 ± 0.76°C large endothermic peak in the temperature range of 54.97 assigned to lignin decomposition, present in all the ± 2.34°C - 69.18 ± 3.45°C, attributed to the elimination species studied. The other transition is between 479.02 of moisture when the sample is heated. The second ± 1.09°C - 542.93 ± 4.56°C; according to other studies, transition is endothermic and is related to the degradation this transition has been related to the formation of of hemicelluloses in the range between 200.40 ± 0.87°C gaseous products released during the pyrolysis process - 200.79 ± 3.98°C and similar values were found in the experienced by the samples. nests of the wasp species studied. The third transition is

Table II. Maximium Temperatures and Enthalpy of Cellulose Obtained from the DSC Curves

The nests of B. lecheguana and A. pallipes had the hi- comparisons with other studies related to thermal analy- ghest temperatures associated with cellulose degradation sis in wood, finding thermal behavior similar to the re- (Table II). Behavior that may be associated with the hi- sults obtained in the nests of the wasp species evaluated gher crystalline cellulose content in these nests [25]. Ce- in this study [19],[27],[28],[29]. llulose enthalpy is also higher in B. lecheguana and A. pallipes compared to the nests of the other species. This is due to the fact that the cellulose chains organized in the nests of these two species can increase the thermal stabi- lity of the material even when the degradation tempera- tures of the extractive content are high (Table 4), since it is necessary to supply more energy to melt the cellulose crystals which increases their enthalpy.

Currently, in the scientific literature, few studies of ther- mal analysis in materials designed by social insects are reported, especially in wasp construction material. The study reported by Erik Schmolz [26], corroborates the results obtained in this study. On the other hand, consi- dering that wasp nests are built using worn wood fibers, it is possible to make Respuestas, 24 (2), pp. 27-38 , 2019, ISSN 0122-820X - E ISSN: 2422-5053 32 María Del Carmen Parra Hernández, Diana Alexandra Torres Sánchez

DSC curves for the nests of the wasp species studied. A) A. pallipes, B) A. multipicta, C) A. areata, D) P. aequatorialis, E) P. apicalis, F) M. imitator, G) B. lecheguana 33 Respuestas, 24 (2), pp. 27-38, 2019, ISSN 0122-820X - E ISSN: 2422-5053 Chemical and thermal characterization of the construction material of nests of seven species of wasps from Norte de Santander - Colombia.

The IR spectra for the nest samples of the seven wasp species can be seen in Figure 3. FTIR-ATR Spectroscopy

FTIR-ATR spectra of nest samples of different species.

Table III. IDENTIFICATION OF FUNCTIONAL GROUPS IN THE IR SPECTRA OF THE SAMPLES

Respuestas, 24 (2), pp. 27-38 , 2019, ISSN 0122-820X - E ISSN: 2422-5053 34 María Del Carmen Parra Hernández, Diana Alexandra Torres Sánchez

Table III lists the respective identification of the Table IV shows the concentration of the metals found in different IR bands in the samples studied; it is possible the samples. The species A. areata records the highest to observe the presence of bands assigned to vibrational values in the metals K, Ca, Al, Mg, Ti, Cr, Mn, Fe, Ni, Zn modes characteristic of methyl, methylene, hydroxyl and Li except for Cu metal in which intermediate values groups characteristic of cellulose, hemicellulose and are recorded in comparison with the other species. While present in many groups of lignin and carbohydrates in the nests of the species B. lecheguana low values are [25],[30],[31]. registered in the concentration of the metals Ca, Mg, Ti, X-ray fluorescence - XRF Cr, Mn and Cu, with respect to the other species of wasps. The metals Fe, Ca and Mg determined coincide with those found in other studies, affirming that the material

CONCLUSIONS to the decomposition of hemicelluloses, the second pro- cess (274,10 ± 4,65 °C - 307,39 ± 1,23 °C) associated The characteristic bands of the compounds, in the FTIR with cellulose degradation and the third process (323,22 spectra of the nests of the different species, exhibit the ± 0,34 °C - 350,95 ± 8,15 °C) corresponding to lignin presence of hemicellulose, cellulose and lignin, as well as degradation. aliphatic and aromatic hydrocarbons, alcohols, phenols, ketones and aliphatic acids. By thermal analysis, it is found that the nests of the spe- cies M. imitator, P. apicalis and A. multipicta have less Through X-ray fluorescence (XRF) were found in all thermal stability compared to the samples of the other samples mostly iron and aluminum, results that differ species, and the building material of these species is from that reported for nests of species not found in Co- characterized by starting the degradation process at re- lombia, which contain more calcium and potassium. latively lower temperatures, which causes a reduction in thermal stability. Behavior that is probably associated Thermogravimetric analysis showed that the nest sam- with a greater volatility of the extracts (low molecular ples of the analyzed species A. pallipes, A. multipicta, weight compounds). A. areata, P. aequatorialis, P. apicalis, M. imitator and B. lecheguana, presented four losses of mass, the first of The results of the different analyses indicate that there these (50.32 ± 0.84 - 87.45± 6.74 °C) attributed to the loss are variables of structure, composition and thermal beha- of water in the form of moisture absorbed in the surface viour that differ significantly in the nests regardless of the of the nest; In addition to this there are three other pro- species, genus or place of origin of the samples. cesses, the first (200,39 ± 2,34 °C - 238,58 ± 1,80 °C) attributed

35 Respuestas, 24 (2), pp. 27-38, 2019, ISSN 0122-820X - E ISSN: 2422-5053 Chemical and thermal characterization of the construction material of nests of seven species of wasps from Norte de Santander - Colombia. can offer very promising applications in adsorption do Parque Estadual do Ibitipoca, Minas Gerais, studies,[32] other authors affirm that the composition of Brazil.,” MG Biota, vol. 3, no. 4, pp. 22–32, the material is quite different from one species to another, 2010. and report that the most important components in the nests are: Ca, Si, Al, Mg and K, this coincides with the results obtained in this study, although the metal found in [7] M. Shah, M. S. Khan, M. A. Rafi, S. A. Mehmood, greater quantity was iron [2],[23]. and M. Farooq, “Nesting biology and Social behaviour of ( flavus) and ACKNOWLEDGEMENTS Honey (Apis mellifera) in District Mansehra, Pakistan,” Int. J. 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