Molar Mass Research Articles

A new semi-empirical correlation for the evaluation of the dynamic viscosity of nanofluids

Thanks to their excellent heat transfer coefficient, nanofluids can be considered as ideal heat transfer fluids for a large number of relevant engineering and scientific applications. Precise assessments of their thermophysical properties are thus essential for reliable calculations. In this work, a new semi-empirical scaled correlation based on 8 parameters (volume fraction, temperature, base fluid critical temperature, base fluid density, base fluid critical density, nanoparticle diameter, base fluid molar mass, nanoparticle density) is introduced to evaluate the dynamic viscosity of nanofluids. The correlation is regressed and evaluated using a dynamic viscosity dataset for 32 nanofluids, including a total of 737 experimental points: 10 nanofluids have water as base fluid (Ag, Al2O3, Al2O3/CuO, C, CuO, diamond, Fe/Si, MWCNT, ND-Ni, TiO2), 6 nanofluids have ethylene glycol (Ag, Al2O3, CeO2, Co3O4, SiC, TiO2/CuO), 11 nanofluids comprise different mixtures of water and ethylene glycol (Al2O3, MWCNT/WO3, CB, fGnP, G/Dp, G/Dr, nD87, nD97, TiO2), 1 nanofluid has propylene glycol (SiC) and 4 nanofluids comprise different mixtures of water and propylene glycol (TiB2, TiB2/B4C, fGnP). The dynamic viscosity dataset was derived from experimental measurements documented in the scientific literature and conducted with samples that were prepared using consistent and reliable methods. The study evaluates the dynamic viscosity of nanofluids using 14 literature equations to verify their accuracy against the proposed correlation. Results show that the correlation has an average absolute relative deviation of 8.16%, which is significantly lower than that of the literature equations. A 4-fold cross-validation also shows that the correlation is resilient and accurate with different regression datasets.

Fabrication of stable hydrogel microspheres with hydrophobic shell using water-in-water (W/W) Pickering emulsion template

Hydrogel microspheres are promising for food applications. The water-in-oil (W/O) emulsion template is commonly used to prepare the hydrogel microspheres. However, this method often involves synthetic surfactants and toxic organic solvents to remove the oil phase. The swelling problem of the resultant microspheres is another obstacle. In this study the water-in-water (W/W) emulsion template of gelatin-in-dextran was used to prepare the hydrogel microspheres, without the addition of surfactants, toxic reagents and high energy input. To prevent swelling, zein particles modified with alginate were served as a hydrophobic shell of the gelatin core. The formation evolution of these core–shell microspheres and its relevant factors including phase behavior of the immiscible gelatin/dextran, the binding of zein/alginate and the addition of the modified zein particles were investigated. It was found that small amount of alginate could induce zein particles to absorb on the gelatin surface, whereas the excess led to absorption competition. When using 0.6 wt% particles with zein/alginate ratio of 1:0.5, the ideal core–shell microspheres which were fully covered by the particles and with a self-supporting architecture in uniform size (18.8 ± 0.1 μm) and spherical shape were obtained. These microspheres showed remarkable stability under the conditions of heat treatment, varied pHs and salt concentrations and long-term storage either in refrigerator or room environment. Their sizes were easily manipulated by adjusting the concentration and molar mass of the biopolymers. It is believed that the desired stability and tunable sizes of these edible core–shell microspheres could contribute the development of their applications in foods.

Poxylated stereocomplexes from PEtOx-b-PLA diblock copolymers

An ω-hydroxyl terminated poly(2-ethyl-2-oxazoline) (PEtOx) was obtained by termination of the cationic ring-opening polymerization of 2-ethyl-2-oxazoline with acetate and subsequent transesterification with methanol. The resulting PEtOx-OH featuring a degree of polymerization (DP) of 20 was used as a macroinitiator for the ring-opening polymerization of l-lactide as well as d-lactide. The resulting PEtOx-b-PLA block copolymers featured DP values of 25, 50, 100 and 150, respectively, and were characterized by means of size exclusion chromatography, 1H NMR spectroscopy as well as matrix-assisted laser desorption ionization mass spectrometry. Differential scanning calorimetry, wide-angle x-ray scattering and polarized light microscopy indicated the formation of stereocomplexes in racemic blends of PEtOx-b-PLA with opposing chirality. Thereby, the amorphous PEtOx block did not affect the modification of the stereocomplex crystallites, as shown by comparison with data obtained from PLA homopolymer stereocomplexes. Similar to those, the degree of crystallinity and melting temperature decreased with increasing molar mass of the PLA in the stereocomplexes formed from PEtOx-b-PLA block copolymers.

Light-Driven Organocatalyzed Controlled Radical Copolymerization of (Perfluoroalkyl)ethylenes and Vinyl Esters/Amides.

Fluoropolymers of well-defined structures exhibit significant potential in a broad range of high-tech applications. However, the controlled synthesis of fluoropolymers from easily available monomers remains difficult. In this work, we report the development of an organocatalyzed controlled radical copolymerization of (perfluoroalkyl)ethylenes (PFAEs) and unconjugated vinyl monomers (UCMs) under light irradiation, which has enabled on-demand access toward side-chain fluorinated polymers under metal-free conditions. This method furnishes a large variety of polymers with diverse fluoroalkyl and ester/amide as pendent groups, tunable molar masses, and low dispersities (ca. Đ = 1.1-1.3), and adjustable fractions of PFAE and UCM units. Obtained fluoropolymers exhibit good chain-end fidelity and activity, allowing chain-extension polymerizations to prepare block copolymers of complicated compositions. Furthermore, the PFAE copolymers exhibit outstanding light transmission and low refractive index.

Thermal behavior of polymers and copolymers based on plant oils with differing saturated and monounsaturated content

AbstractPlant oil‐based acrylic monomers from hydrogenated sunflower (HFM), palm (PMM) and castor (CSM) oils were polymerized to investigate the effect of chemical composition on polymer phase transitions at temperatures relevant to physiological range. While HFM and PMM possess a highly differing content of saturated palmitic and stearic acids combined with unsaturated fatty acids, CSM contains primarily fragments based on monounsaturated ricinoleic hydroxy acid (up to 90%). Differential scanning calorimetry (DSC) measurements indicate that polymers from PMM and HFM are both semicrystalline (with Tm = −6 and −13 °C, respectively), while poly(CSM) appears to be amorphous (Tg = −49 °C). Considering the similarity in polymers' molar mass (Mn = 16 000–20 000 g mol−1), the observed thermal transitions can be explained by the formation of ordered morphological domains due to the presence of saturated palmitic and stearic acid fractions in poly(PMM) and poly(HFM). For copolymers of CSM, PMM and HFM (80 wt% of monomer feed) with styrene, DSC data show two transitions corresponding to the mobility of long alkyl fatty acid side fragments and the macromolecular backbone. For copolymers of PMM and HFM, comparable values (−52.8 and −55.5 °C, respectively) were obtained, while the second transition for poly(CSM‐co‐styrene) appears at 35 °C. We attribute this higher value to the presence of hydroxyl groups in ricinoleic acid fragments of CSM serving as additional chain transfer sites and the formation of macromolecular fractions enriched with polystyrene fragments. We expect that the temperature transitions obtained can be relevant to the future use of these polymers for biomedical applications, including the synthesis of polymer brushes. © 2024 Society of Chemical Industry.

Real-Time Estimation of CO2 Absorption Capacity Using Ionic Conductivity of Protonated Di-Methyl-Ethanolamine (DMEA) and Electrical Conductivity in Low-Concentration DMEA Aqueous Solutions

The present study investigates the real-time estimation of CO2 absorption capacity (CAC) based on the electrical conductivity (EC) of low-concentration di-methyl-ethanolamine (DMEA) solutions (0.1–0.5 M). CO2 absorption experiments are conducted to measure the variation in CAC and EC during CO2 absorption, revealing a strong correlation between the two properties. The ionic conductivity of DMEAH+ formed during absorption is calculated to be 53.1 S·cm2/(mol·z), which is found to be larger than that of TEAH+ and MDEAH+. This can be attributed to the smaller molar mass and higher ionic mobility of DMEAH+. A significant finding is that the measured EC (ECM) of the DMEA solutions consistently demonstrates a lower value than the theoretically predicted value. This discrepancy is due to the larger ionic size of DMEAH+, which results in a reduction in the real mean ionic activity coefficient. This effect becomes more pronounced with increasing DMEA concentration. Consequently, a higher CAC is required to produce the same change in EC at higher amine concentrations. Based on these findings, an empirical equation is devised to estimate CAC from ECM in solutions of constant DMEA concentration. This equation will be employed as a practical approach for the in situ monitoring of CO2 absorption using DMEA aqueous solution.

Synthesis of biobased poly(ether-ester) from potentially bioproduced betulin and p-coumaric acid

For a more sustainable future, innovative polymer materials synthesized from biobased molecules are currently a key trend, in the frame of the bioeconomy. In this study, new renewable macromolecular architectures poly(ether-esters) has been synthesized from betulin and para-coumaric acid, two plant-based building blocks, poorly valorized till now, and potentially bioproduced by white biotechnologies. To date, these are the first synthesized polymers with such a reported architecture. In a first step, different chemical modifications were carried out on these biomolecules to increase their reactivities. Betulin hydroxyl groups were esterified with aliphatic acids of carbon chain lengths C6, C8 and C10 terminated by a bromine, with good yields (79–85%). P-coumaric acid was dimerized by [2 + 2] cycloaddition, and then esterified with ethanol, butanol or isobutanol with excellent yields (92–96%). These modified building blocks were finally copolymerized by Williamson polyetherification reaction, leading to various analogous materials with molar masses ranging from 9700 to 15500 g mol−1. Different thermal characterizations have been then performed. TGA results show that these poly(ether-esters) displayed high thermal stabilities (up to 336 °C). Besides, DSC analyses revealed Tg ranging from 38 to 81 °C, depending on the length of the aliphatic carbon chain and the nature of the pendant ester groups for a large range of potential applications.

Isolation of β-O-4-Rich Lignin From Birch in High Yields Enabled by Continuous-Flow Supercritical Water Treatment.

The continuous flow supercritical water (scH2O) treatment of Birch wood (T=372-382 °C; t=0.3-0.7 s; p=260 bar) followed by alkali extraction of lignin allowed for the isolation of lignin and lignin carbohydrate complexes (LCCs) with a high number of β-O-4 moieties in the range 29-57/100 Ar (evaluated by quantitative 13C NMR analysis) in yields ranging between 13-19 wt % with respect to the initial wood. A "lightning rod effect" of carbohydrates has been claimed to explain the low degradation of β-O-4 bonds during the process. The structure of the isolated lignin was thoroughly elucidated via comprehensive NMR studies (HSQC, 13C and 31P). A low degree of condensation (DC)<5 % was found for all the lignin samples, which was only slightly dependent on the reaction severity. The number of aliphatic -OH, phenolic -OH, and -COOH groups was in the range 3.37-5.25, 1.41-2.31 and 0.39-0.73 mmol/g, respectively. The number of -COOH groups increased with increased severity, suggesting that oxidation can occur during the scH2O treatment. Furthermore, by simply varying the reaction severity, it was possible to tune important lignin properties, like the molar mass and the glass transition temperature (Tg).

Foxtail millet bran dietary fibres foster in vitro beneficial gut microbes and metabolites while suppressing pathobionts

Foxtail millet bran soluble dietary fibre (MBSDF) is a dietary compound with various bioactivities, potentially modulated by the gut microbiota. To elucidate this bioregulatory mechanism, this study focused on the structureal composition and in vitro fermentation characteristics of MBSDF. The results revealed that MBSDF has a molecular weight of 18.26 kDa. The main chain is connected through a glycosidic bond in the form of →4)-α-D-Glcp-(1 → 4)-β-D-Xylp-(1→, being branched by →4, 6)-α-D-Glcp-(1 → O-6 and →3, 4)-β-D-Xylp-(1 → O3 bonds. After 24 h fermentation, the carbohydrate utilisation rate reached 59.15 %, with a decreased molecular weight and monosaccharide composition molar mass ratio. Meanwhile, a increase was observed in the short-chain fatty acid, accompanied by an increased relative abundance of Faecalibacterium, Bifidobacterium and Lactobacillus and suppressed growth of pathogenic Enterococcus. Interestingly, the modulation of gut homeostasis probably occurs via butyrate metabolism pathway. Collectively, MBSDF can selectively regulate the gut microbiota and their metabolites.

Copolymer Randomization by End‐Group Interchain Exchange Reactions

AbstractTheoretical analysis of the kinetic scheme describing formation and randomization of a binary copolymer due to end‐group interchange reactions is presented. Compact analytical expressions are obtained for the transient and equilibrium values of the copolymer degree of blockiness and fractions of active end‐groups of different types. The resulting copolymer is described by the first‐order Markov statistics, which can be rather far from the Bernoullian one. Its structure is determined by the composition of the system and a single combination of the rate constants of four elementary reactions. The kinetics includes fast and slow stages with characteristic time periods independent of and proportional to the average polymerization degree, respectively. During the fast stage, the initial polymers disappear, whereas the copolymer degree of blockiness is still very low. The distribution of units in the copolymer is Markovian, only if the initial polymers possess the most probable molar mass distributions. At the slow stage copolymer randomization gradually progresses, whereas the distribution of end groups may change in the opposite direction compared to the fast stage. The results can be used to analyze the experimental data on the chain structure of condensation, metathesis, and dynamic covalent polymers, where interchange reactions play a significant role.

Impact of electrolyte on the structure and orientation of water at air/water-polyethylene glycol polymer interface.

Polyethylene glycol (PEG) is a water soluble, non-ionic polymer with applications in drug delivery, protein precipitation, anti-biofouling, water-splitting, Li-ion batteries, and fuel cells. The interaction of PEG with water and electrolytes plays pivotal roles in such applications. Using interface-selective spectroscopy, heterodyne-detected vibrational sum frequency generation, and Raman difference spectroscopy with simultaneous curve fitting analysis, we show that water adopts different structures and orientations at the air/water-PEG interface, which depends on the molar mass of the PEG. At the air/water-PEG4000 (MW 4000u) interface, water is H-up oriented (i.e., water Hs are pointed away from the aqueous bulk) around 3200cm-1 and H-down oriented (i.e., water Hs are pointed toward the aqueous bulk) around 3470cm-1. Variation of the bulk concentration of PEG4000 does not change the dual orientation of interfacial water. The presence of an electrolyte (1.0M NaCl) selectively reduces the H-up oriented water without affecting the H-down oriented water at the air/water-PEG4000 interface. The selective reorganization of the interfacial water is assigned to the disruption of the asymmetric hydration around ether-oxygen of the surface-adsorbed PEG4000 by the Na+ ion of the electrolyte. Interestingly, in the case of low molar mass PEG (air/water-PEG200), the interfacial water neither shows the dual orientation nor is affected by 1.0M NaCl.

Flat biofilms extrusion of poly(lactic acid)/poly(butylene adipate‐co‐terephthalate) grafted with glycidyl methacrylate blends: Toward ecological packaging for sustainability

AbstractBlends of poly(lactic acid) (PLA)/poly(butylene adipate‐co‐terephthalate) grafted with glycidyl methacrylate (PBAT‐g‐GMA) were developed to produce flat and flexible biofilms through extrusion. The PLA/PBAT‐g‐GMA (90%/10%, 80%/20%, 70%/30%, and 60%/40% by mass) blends were processed in the internal mixer, injection molded, and manufactured into flat films. The optimal composition to produce flexible biofilms was PLA/PBAT‐g‐GMA (60/40%), as it demonstrated a decrease in elastic modulus of 53.2% and a significant gain in elongation at a break of 4923% about pure PLA. The incorporation of 40% PBAT‐g‐GMA in PLA increased the torque (Z) by 208%, while the melt flow index (MFI) decreased by 51.57%, compared to PLA. Additionally, the degradation rate (Rz) and molar mass loss (Rm) during processing were minimized, indicating that 40% PBAT‐g‐GMA enhanced stability of the PLA matrix. Fourier transform infrared spectroscopy indicated interactions between the GMA of PBAT‐g‐GMA and PLA, justifying the increase in viscosity and elongation at break. The PLA/PBAT‐g‐GMA (60/40%) composition showed a transmittance in the range of 20%–48% (400–800 nm) and an oxygen gas permeability of 1.56 × 10−5 cm3 STP/cm−2 h bar, indicating its potential for applications in packaging with optical barrier properties. Scanning electron microscopy (SEM) revealed ligaments in the interfacial region between PLA and PBAT‐g‐GMA, confirming the good performance in elongation at break. The results presented are essential for the plastics processing sector, aiming to develop eco‐friendly packaging.

Dead Sea water as a sustainable source for the production of microbial bioplastics polyhydroxyalkanoates by halophiles

The Dead Sea is a unique salt-saturated water body. This work utilized the Dead Sea water (DSW) as a medium instead of fresh water for the biosynthesis of polyhydroxyalkanoates (PHAs) by Haloferax mediterranei. The intracellular content of PHAs reached a maximum (6.35 %) at 40 % DSW. An artificial DSW media that mimics the DSW composition was prepared and used for PHAs production by H. mediterranei. The cell dry mass (CDM) and PHAs comcentration (32.61 g L−1 and 4.56 g L−1, respectively) were significantly higher than the results obtained from the reported H. mediterranei highly saline medium. The PHAs production was scaled-up to fed-batch utilizing no-cost date fruit waste and resulted in CDM and PHA concentration of 46.89 g L−1 and 12.77 g L−1, respectively under non-sterile conditions. H. mediterranei accumulated poly-3-(hydroxybutyrate-co-9 %-hydroxyvalerate) with molar mass 916.0 kDa and melting point at 143.2 °C. These results indicate the production of a high-quality biopolymer.

Free radical copolymerization kinetics of bio-based dibutyl itaconate and n-butyl acrylate

The free radical copolymerization of dibutyl itaconate (DBI), a monomer derived from renewable resources, and n-butyl acrylate (BA) is investigated to explore the potential of incorporating itaconate monomers into commercial acrylic resins to enhance the sustainability of coating materials. Batch experiments were conducted at 50 °C and 80 °C, varying initial monomer and initiator concentrations as well as monomer compositions, with proton NMR and size exclusion chromatography used to analyze monomer conversion profiles and polymer molar mass distributions (MMDs). The data were analyzed using a kinetic model developed to guide the experimental studies and estimate key kinetic parameters controlling copolymer composition, polymerization rate and polymer MMDs. The use of the more reactive BA as comonomer significantly increases the conversion and molar mass of the resulting copolymer. Furthermore, semi-batch operating conditions similar to current industrial practice can incorporate a substantial fraction of DBI into acrylic copolymer resins, thus enhancing their sustainability profile.

Synthesis of miktoarm star-shaped polymers with polyoxazoline arms and macrocyclic calix[8]arene branching center

A novel approach to the synthesis of miktoarm star-shaped poly(2-alkyl-2-oxazolines) with calix[8]arene core was developed using a combination of the “core first” (grafting from) and “grafting onto” methods. The star-shaped polymers of A8B8 type with grafted poly(2-ethyl-2-oxazoline) and poly(2-isopropyl-2-oxazoline) arms were obtained using calix[8]arene based multifunctional branching center with sulfonyl chloride initiating moieties and as well as acyl hydrazide termination ones. The polymer structure has been confirmed by 1H NMR spectroscopy and UV spectroscopy. The molar mass characteristics of the samples were determined by size-exclusion chromatographic and light scattering. It was experimentally confirmed that all synthesized polymers had the target arm number, namely 8 or 16. The obtained miktoarm stars were characterized by narrow molar mass distributions, and the polymerization degree of the arms was 15. The synthesized stars had a high intramolecular density, which increased with the arm number. It is shown that the thermoresponsiveness of the studied stars depends on the number and structure of arms and on intramolecular density, while molecular mass is not a decisive factor determining their LCST behavior.For miktoarm stars, phase separation temperatures do not depend on the grafting configuration of poly(2-ethyl-2-oxazoline) and poly(2-isopropyl-2-oxazoline) on the upper or lower rim of calix[8]arene.

Starch digestion and physiochemical properties of a newly developed rice variety with low glycemic index

This study aimed to clarify the starch digestion characteristics and related physicochemical properties of the newly developed low-GI rice variety, Ditangliangyou 335 (D335), in comparison with two widely grown rice varieties, Xiangzaoxian 45 (X45) and Zhongzao 39 (Z39). The results showed that D335 had an active digestion duration (286 min) that was 101–190 % shorter, a glucose production rate (1.06 mg g−1 min−1) that was 57–73 % slower, and a total glucose production (303 mg g−1) that was 11–19 % less than X45 and Z39. These differences were attributable to the distinct starch physicochemical properties, including amylose content, amylose-to-amylopectin ratio, starch granule size, amylopectin chain length, and starch molar mass, as well as the different pasting properties of rice flour, such as pasting temperature and breakdown viscosity. These findings reveal the starch digestion characteristics and the key physicochemical properties that determine these characteristics in the low-GI rice variety D335.

Assessing the potential for upscaling the continuous production of lignin oils through reductive catalytic depolymerization

Lignin represents up to one third of lignocellulosic biomass and is a sustainable carbon source available at a sufficient scale to replace an impactful amount of fossil resources when converted into materials and chemicals. The molecular structure of lignin renders it ideal to obtain renewable aromatic building blocks for the polymer industry. Nevertheless, in polymeric form, lignin poses serious challenges for material applications and chemical conversion, namely poor solubility, and low reactivity. This problem can be circumvented by depolymerization of isolated lignins. To meet the demand for renewable aromatic building blocks, it is crucial to utilize technical lignin streams generated on large scale. This will eventually allow the development of continuous, high-throughput processes which are required for viable industrial-scale operations. Our work demonstrates for the first time that “technical grade” hydrolysis lignin from an operating biorefinery can be successfully subjected to continuous reductive catalytic depolymerization (RCD) in a packed bed reactor using a commercially available Pd/Al2O3 catalyst. The impact of catalyst amount, feed concentration (in methanol), and temperature with regards to process stability and product quality was investigated. The product was characterized by NMR, GPC, and GC-FID. Feed concentrations up to 7 wt% could be continuously processed for 77 h at 200 °C whereas at 225 °C, the operation time was restricted to 21 h. In all cases, a stable output was obtained over time in terms of molar mass, OH-group distributions, and monomer content. At 200 °C, carbon yields above 90 % of the soluble lignin fraction were feasible.

Interlayer engineering of V2O5·nH2O by conductive Ni-BTA enabling high-performance aqueous ammonium ion batteries

Aqueous ammonium ion batteries (AAIBs) are of interest due to the low molar mass, small hydration radius, abundant raw materials and high safety of the carrier ammonium-ion. Nevertheless, there are numerous constraints associated with electrode materials that are suitable for ammonium-ion storage. In this study, we design and synthesize a composite comprising of one-dimensional conductive metal-organic skeleton material (1D c-MOF) embedded between layers of hydrated vanadium pentoxide (VOH) with improved ammonium-ion storage. The central ion of the 1D c-MOF is selected to be the nickel ion, while the ligand is 1,2,4,5-benzenetetramine (BTA). The incorporation of Ni-BTA between the vanadium oxide layers results in the formation of a composite (Ni-BTA/VOH) exhibiting enhanced structural stability, augmented layer spacing and elevated conductivity. Furthermore, the dual energy storage mechanisms of VOH and CN rearrangement act in concert to yield a “1+1 > 2” effect, thereby markedly enhancing the ammonium-ion storage. The specific capacity of Ni-BTA/VOH can reach 183 mAh g−1 at 0.2 A g−1, and the retention rate can reach 52.5 % after 500 cycles at 2 A g−1. This work not only proves the potential of Ni-BTA/VOH for widespread application in the field of aqueous batteries, but also provides a new method for structural engineering of VOH with boosted ammonium-ion storage properties.

Synthesis and thermal characterization of polyesters and copolyesters containing selenium with potential self‐healing behavior

AbstractThis work presents a versatile method for obtaining a new family of selenium‐containing polyesters through polycondensation reactions, focusing on methodology of the synthesis, thermal characterization, and evaluation of potential self‐healing behavior of these structures. Using diselenides as monomers, homopolymers and copolymers with self‐healing behavior were synthesized in good yields and molar masses, and their structural characteristics could be modulated according to the type of monomers and their proportions. In this way, a wide range of polymers were obtained using monomers with aliphatic and aromatic structures. All the synthesized polymers were evaluated in terms of their thermal stability, which reached 200°C, and their completely amorphous structure, where the Tg could be modulated by adjusting the proportion of monomers. In addition, the self‐healing potential of polymers that were able to form films and exhibited structural mobility at room temperature was qualitatively evaluated. After 12 h of exposure to visible light at a controlled temperature, the structures containing aromatic and aliphatic mixtures at a 1:1 ratio were able to regenerate almost 100% of their surface area. The results presented in this work can contribute to the development of new methodologies for obtaining selenium‐containing polymers while increasing the range of possible self‐healing compounds.

Structural, molecular, and physicochemical properties of starch in high-amylose durum wheat lines

There is growing interest in the development of high-amylose cereals such as wheat due to their functional properties and nutritional value in foods. The increase in amylose content is associated with significant changes in the physicochemical, molecular, and structural characteristics of wheat starch which could affect its processing quality. The present study aimed to analyze the physicochemical, molecular, and structural characteristics of high-amylose starch from three durum wheat near isogenic lines (NILs), each obtained using three different recurrent parents. Morphology, granule size distribution, pasting and thermal properties, X-ray diffraction, and structural features were determined. The NILs showed the highest amylose content (65.3 and 69.8%), granules with an elongated shape, size between the wild-type and the mutant, restricted swelling in the pasting profile, the highest average and final gelatinization temperature, and B-polymorphism. The starches from the NILs showed the highest molar mass of amylopectin (AP) (7.0–7.6 × 107 Da) and the lowest amylose (AM) (1.1–1.8 × 106 Da), an issue associated with the biosynthesis of both components. The study on the debranched sample by high-performance size-exclusion chromatography showed that the high-amylose starch had the highest content of long B2 and B3 chains of AP (23.9–26.6%), which was corroborated with the high-performance anion-exchange chromatography analysis where the chains with degree of polymerization >37 had the highest content (18.3–19.1%). The PC1 is highly associated with the MwAM and the AM fraction in the debranched starch analyzed by HPSEC. Characterizing high-amylose durum wheat starch provides information to determine the structure-function relationship and design strategies to produce crosses with structural characteristics of AM and AP for specific applications.