All the solvents and reagents are of high purity and have been purchased commercially from Sigma-Aldrich, Fluorochem, Alfa Aesar and Fisher Scientific. Melting points were recorded using a Gallen kamp melting point apparatus and are uncorrected. 1H and 13C NMR analyses were performed on a 400 MHz spectrometer (Bruker) equipped with a SampleXpress (from Bruker) auto sampler system, using deuterated solvents for the preparation of the samples. The obtained spectra were analyzed using Topspin 7.1 software (Bruker). The chemical shifts were reported in ppm values relative to tetramethylsilane (TMS), used as internal standard. Signals were identified and described as singlet (s), doublet (d), triplet (t) and multiplet (m). Coupling constants were reported in Hertz (Hz). Mass Spectra (ESI), HRMS Agilent technologies 6890N and an inert mass selective detector 5973 mass spectrometer Technologies. Glassware used was dried in a UN55 oven (Memmert) at 200 °C35 (link). Fourier transform Infrared (FTIR) spectrum of the synthesized compounds was taken using KBr pellet press method by Bruker TENSOR 27 FTIR spectrophotometer and the (%) yields are calculated on the basis of 1.0 mM of each reactant used. The synthesized motifs 3(a–u) were characterized as given below:
Un55 oven
Manufactured by Memmert
Sourced in Germany
The Memmert UN55 oven is a convection oven designed for general laboratory applications. It features a stainless steel interior, a mechanical timer, and temperature control up to 300°C. The oven has a volume of 53 liters.
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4 protocols using un55 oven
1
Synthesis and Characterization of Novel Motifs
2
Cocoa Shell Charcoal Production
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The
cocoa skin that was used had a yellow color. Then the cocoa skin was
cleaned from any attached impurities, such as seeds and fruit flesh.
After that, the cocoa shells were cut into small pieces and then dried
under sunlight until dry (moisture content <8%). Then charcoal
was made by carbonization using an MEMMERT UN55 oven (Germany) at
1500 °C for 1 h. After becoming charcoal, the cocoa shells were
crushed using a mortar. The crushed cocoa shells were then sieved
using a 74 m (200 mesh) sieve.
cocoa skin that was used had a yellow color. Then the cocoa skin was
cleaned from any attached impurities, such as seeds and fruit flesh.
After that, the cocoa shells were cut into small pieces and then dried
under sunlight until dry (moisture content <8%). Then charcoal
was made by carbonization using an MEMMERT UN55 oven (Germany) at
1500 °C for 1 h. After becoming charcoal, the cocoa shells were
crushed using a mortar. The crushed cocoa shells were then sieved
using a 74 m (200 mesh) sieve.
3
Forage Harvest Timing and Intercropping Effects
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Three forage harvest timings were evaluated, with each harvest, both in sole crops and intercrops, conducted at the start of the earing stage for H. marinum. Concurrently, the harvest for M. sativa was performed at the initiation of the earing stage, as indicated by Bacchi et al. [30 (link)]. Biomass yield was assessed post-harvest for each plot by cutting approximately 5 cm above the ground level. After segregating the plants for analyzing morphological traits across different treatments, they were uprooted, and the soil surrounding the roots was washed away. The plants were then divided into root, stem, and leaf samples. Measurements for each species included the number of axes (NA), length of stems (LS, cm), and root length (LR, cm). Additionally, counts were made for the number of healthy leaves (NHL) and yellow leaves (NYL). The fresh weight of aerial parts and roots was recorded, followed by drying at 60 °C for 48 h in a Memmert UN55 oven, Germany. Subsequently, the dry matter and its constituents (leaves and roots) were determined.
4
Protein-Based Superabsorbent Matrix Fabrication
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Protein-based samples were obtained following a two-stage process: Initially, PPP and glycerol blends were obtained at three different ratios (50/50, 75/25, and 100/0) by using a two-blade counter-rotating Haake Polylab QC batch mixer (ThermoHaake, Karlsruhe, Germany). Blends were obtained at room temperature and 50 rpm for 5 min; subsequently, protein-based samples were obtained after the processing of blends by the Minijet Piston Injection Molding System (ThermoHaake, Karlsruhe, Germany). Cylindrical specimens (10 mm diameter, 15 mm length) were obtained at 60 • C and 500 bar pressure for 150 s [17] . Superabsorbent matrices were generated after submitting protein-based samples to 48 h of water immersion and subsequent drying either in a conventional oven or by freezedrying. On the one hand, the samples were placed in a UN55 oven (Memmert, Germany) at 50 • C for 24 h. Samples were subjected to heat-drying under natural convection conditions (in the absence of any forced air circulation). On the other hand, the samples were first conveniently frozen at -40 • C for 24 h in a static freezer (Model EVF 110/45; Equitec, Madrid, Spain), and then they were freeze-dried in vacuum flasks fitted to an 8-port manifold of a LyoQuest freeze-dryer (Telstar Technologies, Barcelona, Spain) (condenser temperature: -85 • C; temperature of sample holder: room temperature; pressure: 0.01 mbar).
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