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Cavalcante, L. L., Barbolini, N., Bacsik, Z. & Vajda, V. (2023). Analysis of fossil plant cuticles using vibrational spectroscopy: A new preparation protocol. Review of Palaeobotany and Palynology, 316, Article ID 104944.
Open this publication in new window or tab >>Analysis of fossil plant cuticles using vibrational spectroscopy: A new preparation protocol
2023 (English)In: Review of Palaeobotany and Palynology, ISSN 0034-6667, E-ISSN 1879-0615, Vol. 316, article id 104944Article in journal (Refereed) Published
Abstract [en]

Analyses for organic fingerprints on fossilized plant cuticles and pollen hold valuable chemotaxonomic and palaeoclimatic information, and are thus becoming more utilized by palaeobotanists. Plant cuticle and pollen composition are generally analyzed after standard treatments with several chemical reagents for mineral and mesophyll removal. However, the potential alterations on the fossil composition caused by the different cleaning reagents used are still poorly understood. We tested the effects of commonly used palaeobotanical processing methods on the spectra of fossilized cuticles from successions of Late Triassic to Early Jurassic age, including the gymnosperms Lepidopteris , Ginkgoites , Podozamites , Ptilozamites and Pterophyllum astartense. Our study shows that standard chemical processing caused chemical alterations that might lead to erroneous interpretation of the infrared (IR) spectra. The difference in pH caused by HCl induces changes in the proportion between the two bands at similar to 1720 and 1600 cm(-1) (carboxylate and C-C stretch of aromatic compounds) indicating that the band at similar to 1610 cm(-1) at least partially corresponds to carboxylate instead of C-C stretch of aromatic compounds. Interestingly, despite being used in high concentration, HF did not cause changes in the chemical composition of the cuticles. The most alarming changes were caused by the use of Schulze's solution, which resulted in the addition of both NO2 and (O)NO2 compounds in the cuticle. Consequently, a new protocol using H2CO3 , HF, and H2O2 for preparing fossil plant cuticles aimed for chemical analyses is proposed, which provides an effective substitute to the conventional methods. In particular, a less aggressive and more sustainable alternative to Schulze's solution is shown to be hydrogen peroxide, which causes only minor alteration of the fossil cuticle's chemical composition. Future work should carefully follow protocols, having in mind the impacts of different solutions used to treat leaves and other palaeobotanical material such as palynomorphs with aims to enable the direct comparison of spectra obtained in different studies.

Keywords
Fossil cuticle, Schulze's solution, Hydrogen peroxide, Micro-FTIR, Carbonic acid
National Category
Biological Sciences Earth and Related Environmental Sciences
Identifiers
urn:nbn:se:su:diva-221305 (URN)10.1016/j.revpalbo.2023.104944 (DOI)001046714800001 ()2-s2.0-85165320708 (Scopus ID)
Available from: 2023-09-19 Created: 2023-09-19 Last updated: 2023-09-19Bibliographically approved
Fijoł, N., Mautner, A., Svensson Grape, E., Bacsik, Z., Inge, A. K. & Mathew, A. P. (2023). MOF@Cell: 3D printed biobased filters anchored with a green metal–organic framework for effluent treatment. Journal of Materials Chemistry A, 11(23), 12384-12394
Open this publication in new window or tab >>MOF@Cell: 3D printed biobased filters anchored with a green metal–organic framework for effluent treatment
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2023 (English)In: Journal of Materials Chemistry A, ISSN 2050-7488, E-ISSN 2050-7496, Vol. 11, no 23, p. 12384-12394Article in journal (Refereed) Published
Abstract [en]

Multifunctional, biobased materials processed by means of additive manufacturing technology can behighly applicable within the water treatment industry. This work summarizes a scalable and sustainablemethod of anchoring a green metal–organic framework (MOF) SU-101 onto the surface of 3D printed,biobased matrices built of polylactic acid (PLA)-based composites reinforced with TEMPO-oxidizedcellulose nanofibers (TCNFs). The two tested anchoring methods were hydrolysis via either concentratedhydrochloric acid treatment or via a photooxidation reaction using UV–ozone treatment. Stabledeposition of SU-101 distributed homogenously over the filter surface was achieved and confirmed byFT-IR, XPS and SEM measurements. The obtained 3D printed and functionalized MOF@PLA andMOF@TCNF/PLA (aka MOF@Cell) filters exhibit high efficiency in removing heavy metal ions from mineeffluent and methylene blue from contaminated water, as demonstrated through batch adsorptionexperiments. In addition to their potential for removal of contaminants from water, the MOF@Cell filtersalso exhibit excellent mechanical properties with a Young's modulus value of about 1200 MPa,demonstrating their potential for use in practical water treatment applications. The MOF@Cell filterswere able to maintain their structural integrity and filtration performance even after multiple cycles ofuse and regeneration. This study highlights the potential of multifunctional, biobased materials processedby additive manufacturing technology as a cost-effective alternative to traditional water treatmentmethods. The MOF@Cell filters presented in this study demonstrate high efficiency, durability, andreusability, making them promising candidates for practical applications in the modern water treatmentindustry.

Keywords
Metal ion removal, dye removal, 3D printing, polylactic acid, nanocellulose, metal-organic framework
National Category
Materials Chemistry
Research subject
Materials Chemistry
Identifiers
urn:nbn:se:su:diva-219217 (URN)10.1039/d3ta01757e (DOI)000999466800001 ()2-s2.0-85164153001 (Scopus ID)
Funder
Knut and Alice Wallenberg Foundation, Wallenberg Wood Science CentreSwedish Foundation for Strategic Research
Available from: 2023-07-17 Created: 2023-07-17 Last updated: 2023-12-18Bibliographically approved
Kausar, H., Bacsik, Z. & Hedin, N. (2023). Ultramicroporous polyureas synthesized with amines and 1,1′-Carbonyldiimidazole and their CO2 adsorption. Materials Chemistry and Physics, 296, Article ID 127283.
Open this publication in new window or tab >>Ultramicroporous polyureas synthesized with amines and 1,1′-Carbonyldiimidazole and their CO2 adsorption
2023 (English)In: Materials Chemistry and Physics, ISSN 0254-0584, E-ISSN 1879-3312, Vol. 296, article id 127283Article in journal (Refereed) Published
Abstract [en]

Microporous polyureas can be highly stable, but isocyanates or phosgene are normally used for the synthesis. Here, it was postulated and demonstrated that 1,1′-carbonyl diimidazole (CDI) could be used for the synthesis. By reacting tetrakis(4-aminophenyl)methane with CDI, a series of new polyureas with ultramicropores (pores <0.7 nm) were synthesized. To tailor thermal properties and porosity, the ratio of tetraamine-to-CDI and the reaction temperature were varied. The CO2 adsorption capacities (with values up to 0.74 mmol/g at 0.15 bar/273 K and 1.91 mmol/g at 1 bar/273 K) were ascribed to the ultramicroporosity. The CO2-based Dubinin-Radushkevich surface areas reached 395 m2/g (at 273 K), while the N2-based BET surface areas (at 77 K) were small. The apparent CO2-over-N2 selectivity was also high for the polymers at 273 K with estimated values of 31–92 for 15/85 v/v mixtures of CO2 and N2. This high selectivity was ascribed to the kinetic hindrance of N2 diffusion. It was noted that one of the polymers changed color irreversibly upon heating. In conclusion, it was shown that CDI and amines could be used to synthesize ultramicroporous polyureas, and that these polymers can exhibit irreversible thermochromism. This thermal effect was attributed to the electron-rich urea moieties, aromatic units, and conjugation.

Keywords
1, 1′-carbonyl diimidazole, Urea-linked, CO2/N2 selectivity, Ultramicropores, Thermochromism
National Category
Materials Engineering
Identifiers
urn:nbn:se:su:diva-215290 (URN)10.1016/j.matchemphys.2022.127283 (DOI)000920831600001 ()2-s2.0-85145782103 (Scopus ID)
Available from: 2023-03-14 Created: 2023-03-14 Last updated: 2023-03-14Bibliographically approved
Ménard, D., Blaschek, L., Kriechbaum, K., Lee, C. C., Serk, H., Zhu, C., . . . Pesquet, E. (2022). Plant biomechanics and resilience to environmental changes are controlled by specific lignin chemistries in each vascular cell type and morphotype. The Plant Cell, 34(12), 4877-4896
Open this publication in new window or tab >>Plant biomechanics and resilience to environmental changes are controlled by specific lignin chemistries in each vascular cell type and morphotype
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2022 (English)In: The Plant Cell, ISSN 1040-4651, E-ISSN 1532-298X, Vol. 34, no 12, p. 4877-4896Article in journal (Refereed) Published
Abstract [en]

The biopolymer lignin is deposited in the cell walls of vascular cells and is essential for long-distance water conduction and structural support in plants. Different vascular cell types contain distinct and conserved lignin chemistries, each with specific aromatic and aliphatic substitutions. Yet, the biological role of this conserved and specific lignin chemistry in each cell type remains unclear. Here, we investigated the roles of this lignin biochemical specificity for cellular functions by producing single cell analyses for three cell morphotypes of tracheary elements, which all allow sap conduction but differ in their morphology. We determined that specific lignin chemistries accumulate in each cell type. Moreover, lignin accumulated dynamically, increasing in quantity and changing in composition, to alter the cell wall biomechanics during cell maturation. For similar aromatic substitutions, residues with alcohol aliphatic functions increased stiffness whereas aldehydes increased flexibility of the cell wall. Modifying this lignin biochemical specificity and the sequence of its formation impaired the cell wall biomechanics of each morphotype and consequently hindered sap conduction and drought recovery. Together, our results demonstrate that each sap-conducting vascular cell type distinctly controls their lignin biochemistry to adjust their biomechanics and hydraulic properties to face developmental and environmental constraints. 

National Category
Biological Sciences
Identifiers
urn:nbn:se:su:diva-210649 (URN)10.1093/plcell/koac284 (DOI)000922798100019 ()36215679 (PubMedID)
Available from: 2022-10-25 Created: 2022-10-25 Last updated: 2023-02-28Bibliographically approved
Jasso-Salcedo, A. B., Wang, X., Bacsik, Z. & Hedin, N. (2021). Synthesis of SAPO-56 using N,N,N',N'-tetramethyl-1,6-hexanediamine and co-templates based on primary, secondary, and tertiary amines. Inorganica Chimica Acta, 525, Article ID 120443.
Open this publication in new window or tab >>Synthesis of SAPO-56 using N,N,N',N'-tetramethyl-1,6-hexanediamine and co-templates based on primary, secondary, and tertiary amines
2021 (English)In: Inorganica Chimica Acta, ISSN 0020-1693, E-ISSN 1873-3255, Vol. 525, article id 120443Article in journal (Refereed) Published
Abstract [en]

Biomethane is a renewable fuel with a small environmental footprint. In its production, the removal of CO2 from the fermentation gas is critical. Pressure and vacuum swing adsorption (PSA and VSA) processes have certain advantages over other processes for the removal. Silicoaluminophosphate-56 (SAPO-56) has promising properties as an adsorbent for PSA- or VSA-based upgrading of raw biogas. It is typically synthesized by using N,N,N', N'-tetramethyl-1,6-hexanediamine (TMHD) as a structure directing agent (SDA). In this study, TMHD was partly replaced with three different low-cost templates: isopropylamine (IPA), dibutylamine, and tripropylamine. SAPO-56 was co-crystallized with mixtures of templating amines with up to a ratio of 30%:70% of TMHD:IPA. With using TMHD and IPA, small and defined crystals of SAPO-56 plus SAPO-47 formed instead of the large aggregates of SAPO-56 that formed when only TMHD was used. Solid-state 13C NMR spectroscopy was used to show that the IPA and TMHD had not been decomposed and that both molecules were included within the assynthesized crystals of SAPO-56. Synthetic composition diagrams were drawn with respect to the P2O5, SiO2, and Al2O3 compositions of the reaction mixtures and the formed crystalline SAPOs. In relation to these diagrams, the domains for stability of SAPO-56 were contrasted with those of SAPO-11, -17, -20, and -47. In particular, it was observed that SAPO-47 co-crystallized with SAPO-56 when a very large fraction of IPA was used under otherwise optimized conditions. As consistent with other studies, the SAPO-56 synthesized with dual SDAs had a very high uptake of CO2 at conditions relevant for PSA- or VSA-driven upgrading of raw biogas into methane.

National Category
Chemical Sciences
Identifiers
urn:nbn:se:su:diva-196853 (URN)10.1016/j.ica.2021.120443 (DOI)000675723400004 ()
Available from: 2021-09-20 Created: 2021-09-20 Last updated: 2022-02-25Bibliographically approved
Blaschek, L., Nuoendagula, N., Bacsik, Z., Kajita, S. & Pesquet, E. (2020). Determining the Genetic Regulation and Coordination of Lignification in Stem Tissues of Arabidopsis Using Semiquantitative Raman Microspectroscopy. ACS Sustainable Chemistry and Engineering, 8(12), 4900-4909
Open this publication in new window or tab >>Determining the Genetic Regulation and Coordination of Lignification in Stem Tissues of Arabidopsis Using Semiquantitative Raman Microspectroscopy
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2020 (English)In: ACS Sustainable Chemistry and Engineering, E-ISSN 2168-0485, Vol. 8, no 12, p. 4900-4909Article in journal (Refereed) Published
Abstract [en]

Lignin is a phenolic polymer accumulatig in the cell walls of specific plant cell types to confer unique properties such as hydrophobicity, mechanical strengthening, and resistance to degradation. Different cell types accumulate lignin with specific concentration and composition to support their specific roles in the different plant tissues. Yet the genetic mechanisms controlling lignin quantity and composition differently between the different lignified cell types and tissues still remain poorly understood. To investigate this tissue-specific genetic regulation, we validated both the target molecular structures as well as the linear semi-quantitative capacity of Raman microspectroscopy to characterize the total lignin amount, S/G ratio, and coniferyl alcohol content in situ directly in plant biopsies. Using the optimized method on stems of multiple lignin biosynthesis loss-of-function mutants revealed that the genetic regulation of lignin is tissue specific, with distinct genes establishing nonredundant check-points to trigger specific compensatory adjustments affecting either lignin composition and/or cell wall polymer concentrations.

Keywords
Raman microspectroscopy, Lignin biosynthesis, Semiquantitative in situ analysis, Tissular regulation, Plant biomass, Genetic engineering, Green & Sustainable Science & Technology
National Category
Chemical Sciences Biological Sciences
Identifiers
urn:nbn:se:su:diva-181744 (URN)10.1021/acssuschemeng.0c00194 (DOI)000526592900022 ()
Available from: 2020-05-27 Created: 2020-05-27 Last updated: 2022-05-11Bibliographically approved
Cheung, O., Bacsik, Z., Fil, N., Krokidas, P., Wardecki, D. & Hedin, N. (2020). Selective Adsorption of CO2 on Zeolites NaK-ZK‑4 with Si/Al of 1.8−2.8. ACS Omega, 5(39), 25371-25380
Open this publication in new window or tab >>Selective Adsorption of CO2 on Zeolites NaK-ZK‑4 with Si/Al of 1.8−2.8
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2020 (English)In: ACS Omega, E-ISSN 2470-1343, Vol. 5, no 39, p. 25371-25380Article in journal (Refereed) Published
Abstract [en]

Zeolites with appropriately narrow pore apertures can kinetically enhance the selective adsorption of CO2 over N2. Here, we showed that the exchangeable cations (e.g., Na+ or K+) on zeolite ZK-4 play an important role in the CO2 selectivity. Zeolites NaK ZK-4 with Si/Al = 1.8–2.8 had very high CO2 selectivity when an intermediate number of the exchangeable cations were K+ (the rest being Na+). Zeolites NaK ZK-4 with Si/Al = 1.8 had high CO2 uptake capacity and very high CO2-over-N2 selectivity (1190). Zeolite NaK ZK-4 with Si/Al = 2.3 and 2.8 also had enhanced CO2 selectivity with an intermediate number of K+ cations. The high CO2 selectivity was related to the K+ cation in the 8-rings of the α-cage, together with Na+ cations in the 6-ring, obstructing the diffusion of N2 throughout the zeolite. The positions of the K+ cation in the 8-ring moved slightly (max 0.2 Å) toward the center of the α-cage upon the adsorption of CO2, as revealed by in situ X-ray diffraction. The CO2-over-N2 selectivity was somewhat reduced when the number of K+ cations approached 100%. This was possibly due to the shift in the K+ cation positions in the 8-ring when the number of Na+ was going toward 0%, allowing N2 diffusion through the 8-ring. According to in situ infrared spectroscopy, the amount of chemisorbed CO2 was reduced on zeolite ZK-4s with increasing Si/Al ratio. In the context of potential applications, a kinetically enhanced selection of CO2 could be relevant for applications in carbon capture and bio- and natural gas upgrading.

National Category
Chemical Sciences
Identifiers
urn:nbn:se:su:diva-187870 (URN)10.1021/acsomega.0c03749 (DOI)000580485600043 ()33043217 (PubMedID)
Available from: 2021-01-07 Created: 2021-01-07 Last updated: 2022-02-25Bibliographically approved
Guo, H., Jaworski, A., Ma, Z., Slabon, A., Bacsik, Z., Nedumkandathil, R. & Häussermann, U. (2020). Trapping of different stages of BaTiO3 reduction with LiH. RSC Advances, 10(58), 35356-35365
Open this publication in new window or tab >>Trapping of different stages of BaTiO3 reduction with LiH
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2020 (English)In: RSC Advances, E-ISSN 2046-2069, Vol. 10, no 58, p. 35356-35365Article in journal (Refereed) Published
Abstract [en]

We investigated the hydride reduction of tetragonal BaTiO3 using LiH. The reactions employed molar H : BaTiO3 ratios of 1.2, 3, and 10 and variable temperatures up to 700 °C. The air-stable reduced products were characterized by powder X-ray diffraction (PXRD), scanning electron microscopy, thermogravimetric analysis (TGA), X-ray fluorescence (XRF), and 1H magic-angle spinning (MAS) NMR spectroscopy. Effective reduction, as indicated by the formation of dark blue to black colored, cubic-phased, products was observed at temperatures as low as 300 °C. The product obtained at 300 °C corresponded to oxyhydride BaTiO∼2.9H∼0.1, whereas reduction at higher temperatures resulted in simultaneous O defect formation, BaTiO2.9−xH0.1□x, and eventually – at temperatures above 450 °C – to samples void of hydridic H. Concomitantly, the particles of samples reduced at high temperatures (500–600 °C) display substantial surface alteration, which is interpreted as the formation of a TiOx(OH)y shell, and sintering. Diffuse reflectance UV-VIS spectroscopy shows broad absorption in the VIS-NIR region, which is indicative of the presence of n-type free charge carriers. The size of the intrinsic band gap (∼3.2 eV) appears only slightly altered. Mott–Schottky measurements confirm the n-type conductivity and reveal shifts of the conduction band edge in the LiH reduced samples. Thus LiH appears as a versatile reagent to produce various distinct forms of reduced BaTiO3 with tailored electronic properties.

National Category
Inorganic Chemistry
Research subject
Inorganic Chemistry
Identifiers
urn:nbn:se:su:diva-194826 (URN)10.1039/d0ra07276a (DOI)000573815400041 ()
Available from: 2021-07-08 Created: 2021-07-08 Last updated: 2022-09-15Bibliographically approved
Hao, W., Liu, Y., Neagu, A., Bacsik, Z., Tai, C.-W., Shen, Z. & Hedin, N. (2019). Core-Shell and Hollow Particles of Carbon and SiC Prepared from Hydrochar. Materials, 12(11), Article ID 1835.
Open this publication in new window or tab >>Core-Shell and Hollow Particles of Carbon and SiC Prepared from Hydrochar
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2019 (English)In: Materials, ISSN 1996-1944, E-ISSN 1996-1944, Vol. 12, no 11, article id 1835Article in journal (Refereed) Published
Abstract [en]

The applications of silicon carbide (SiC) include lightweight materials with thermal shock resistance. In this study, core-shell C-SiC particles were synthesized by compacting and rapidly heating a hydrochar from glucose by using strong pulsed currents and infiltration of silicon vapor. Hollow particles of SiC formed on removing the carbon template. In contrast to related studies, we detected not only the pure 3C polytype (-SiC) but also significant amounts of the 2H or the 6H polytypes (-SiC) in the SiC.

Keywords
hollow spheres, silicon carbide, hydrothermal carbonization, pulse current treatment, silicon infiltration
National Category
Materials Engineering Chemical Sciences
Identifiers
urn:nbn:se:su:diva-170875 (URN)10.3390/ma12111835 (DOI)000472638600109 ()31174261 (PubMedID)
Available from: 2019-07-23 Created: 2019-07-23 Last updated: 2022-03-23Bibliographically approved
Rzepka, P., Bacsik, Z., Pell, A. J., Hedin, N. & Jaworski, A. (2019). Nature of Chemisorbed CO2 in Zeolite A. The Journal of Physical Chemistry C, 123(35), 21497-21503
Open this publication in new window or tab >>Nature of Chemisorbed CO2 in Zeolite A
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2019 (English)In: The Journal of Physical Chemistry C, ISSN 1932-7447, E-ISSN 1932-7455, Vol. 123, no 35, p. 21497-21503Article in journal (Refereed) Published
Abstract [en]

Formation of CO32- and HCO3- species without the participation of the framework-bridging oxygen atoms (-O-) upon chemisorption of CO2 in zeolite vertical bar Na-12 vertical bar-A is revealed. The transfer of O and H atoms is very likely to have proceeded via the involvement of residual H2O or -OH groups. A combined study by the solid-state H-1 and C-13 MAS NMR, quantum chemical calculations, and in situ infrared spectroscopy showed that the chemisorption mainly occurred by the formation of HCO3-. However, at a low surface coverage of physisorbed and acidic CO2, a significant fraction of HCO3- was deprotonated and transformed into CO32-. We expect that a similar chemisorption of CO2 would occur for low-silica zeolites and other basic silicates of interest for capture of CO2 from the gas mixtures.

National Category
Chemical Sciences Chemical Engineering
Identifiers
urn:nbn:se:su:diva-174874 (URN)10.1021/acs.jpcc.9b04142 (DOI)000484882500020 ()
Available from: 2019-10-14 Created: 2019-10-14 Last updated: 2022-02-26Bibliographically approved
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