FEATURES OF THE STATION OF STARCH OF N-(3-CHLORO-2-HYDROXYPROPYL)-N,N,N-TRIMETHYLMONONY CHLORIDE

Author(s):  
В.В. ЛИТВЯК

Исследованы особенности катионизации картофельного крахмала N-(3-хлоро-2-гидроксипропил)-N,N,N-триметиламмоний хлоридом (ХГПТМАХ). В качестве методов исследования применяли фотографирование (макросъемку), ЯМР- и ИК-спектроскопию, рентгенографию для исследования фазовой структуры. Проведены фазовый и гравиометрический анализ и представлены расчеты степени кристалличности (СК) и степени аморфности образцов нативного и катионного картофельного крахмала. При исследовании особенностей химического строения полученного катионного картофельного крахмала со степенью замещения 0,042 выявлено присутствие остатков α-D-глюкопиранозы и ХГПТМАХ, что свидетельствует об изменении аморфно-кристаллической структуры. Установлено существенное уменьшение СК картофельного крахмала после его катионизации при температурах, приводящих к сильному набуханию крахмальных гранул в реакционной смеси. Эти изменения тем значительнее, чем выше температура реакции. Введение в макромолекулу крахмала катионных групп оказывает существенное влияние на термические характеристики крахмала, особенно на начальную температуру и механизм деградации. Features of cationization potato starch N-(3-chloro-2-hydroxypropyl)-N,N,N-trimethylammonium chloride (CHPTMAC) is investigated. Photography (macro photography), NMR- and IR-spectroscopy, x-ray for the study of the phase structure were used as research methods. Phase and gravimetrical analyses carried out and calculations of crystallinity degree (CD) and of amorphousness degree of the samples of native and cationic potato starch are presented. In the study of the chemical structure of the obtaining cationic potato starch with a degree of substitution of 0,042 the presence of residues of α-D-glucopyranose and CHPTMAC revealed that indicates a change in the amorphous crystal structure. A significant decrease in the CD of potato starch after its cation at temperatures leading to a strong swelling of starch granules in the reaction mixture was established. These changes are more significant, the higher the reaction temperature. The introduction in the macromolecule of starch cationic groups has a significant impact on the thermal characteristics of starch, especially on the initial temperature and degradation mechanism.

Author(s):  
Jean-Claude Jésior ◽  
Roger Vuong ◽  
Henri Chanzy

Starch is arranged in a crystalline manner within its storage granules and should thus give sharp X-ray diagrams. Unfortunately most of the common starch granules have sizes between 1 and 100μm, making them too small for an X-ray study on individual grains. There is only one instance where an oriented X-ray diagram could be obtained on one sector of an individual giant starch granule. Despite their small size, starch granules are still too thick to be studied by electron diffraction with a transmission electron microscope. The only reported study on starch ultrastructure using electron diffraction on frozen hydrated material was made on small fragments. The present study has been realized on thin sectioned granules previously litnerized to improve the signal to noise ratio.Potato starch was hydrolyzed for 10 days in 2.2N HCl at 35°C, dialyzed against water until neutrality and embedded in Nanoplast. Sectioning was achieved with a commercially available low-angle “35°” diamond knife (Diatome) after a very carefull trimming and a pre-sectioning with a classical “45°” diamond knife. Sections obtained at a final sectioning angle of 42.2° (compared with the usual 55-60°) and at a nominal thickness of 900Å were collected on a Formvar-carbon coated grid. The exact location of the starch granules in their sections was recorded by optical microscopy on a Zeiss Universal polarizing microscope (Fig. 1a). After rehydration at a relative humidity of 95% for 24 hours they were mounted on a Philips cryoholder and quench frozen in liquid nitrogen before being inserted under frozen conditions in a Philips EM 400T electron microscope equipped with a Gatan anticontaminator and a Lhesa image intensifier.


Synlett ◽  
2021 ◽  
Author(s):  
Hong-Wu Zhao ◽  
Xiao-Fan Bi ◽  
Hai-Liang Pang ◽  
Zhe Tang ◽  
Heng Zhang ◽  
...  

In the presence of Na2CO3, the conjugate addition between α-halogeno hydrazones and nitroso compounds proceeded readily, thus delivering multifunctionalized nitrones in the reasonable chemical yields with excellent strereoselectivities. The chemical structure and stereochemical configuration of title chemical entities were unambiguously identified by an X-ray single crystal structure analysis.


2018 ◽  
Vol 5 (1) ◽  
pp. 39
Author(s):  
Ridhawati Ridhawati ◽  
Abdul Wahid Wahab ◽  
Nursiah La Nafie ◽  
Indah Raya

Mesoporous silica SBA-15 is an interesting material having highly ordered nanopores and large surface area, which is synthesized by sol gel and hydrothermal methods. In this study, mesoporous silica SBA-15 was synthesised with two different methods and the characteris was using X-Ray Diffraction (XRD) and Differential Scanning Calorimetry (DSC). SBA-15 was prepared TEOS as precursor and Pluronic 123 as surfactant. Thermoporous mesoporous DSC thermogram results of the SBA-15A mesoporous silica is (Tg 79oC and Tc 158oC). This is relatively lower than SBA-15B (Tg 86oC and Tc 158oC). The measurement of low angle X-Ray Diffraction SBA-15A has a crystal size 9.46 nm and SBA-15B has a crystal size 9.96 nm. The synthesis of SBA-15 using the hydrothermal method needs to be studied further to obtain thermal characteristics and a more stable crystal structure


Author(s):  
Feng Chuanxing ◽  
Wang Qi ◽  
Li Hui ◽  
Zhou Quancheng ◽  
Meng Wang

AbstractSince materials are the substantial foundation for 3D printing, the lack of theoretical research on 3D printing food materials restricts the development of 3D printing in food field. Based on the principle of 3D starch gelatinization printing, this study revealed the effects of pea protein on the printability of potato starch-based 3D printing materials in granular structure, crystalline structure, chemical structure, textural properties, and thermal properties, through scanning electron microscope, X-ray diffraction, Fourier-transformed infrared, differential scanning calorimetry, and textural method, and developed new food materials for 3D printing. The study indicated the structural properties and physicochemical properties changed regularly with the increase in the content of pea protein, when the content of pea protein was 1%, the printing quality was best. The study provides a new theory for the application of 3D printing in food production and technical support for actual production.


2015 ◽  
Vol 17 (4) ◽  
pp. 65-73 ◽  
Author(s):  
Lucyna Słomińska ◽  
Roman Zielonka ◽  
Leszek Jarosławski ◽  
Aldona Krupska ◽  
Andrzej Szlaferek ◽  
...  

Abstract Air dry potato starch (84.9% d.s.) was subjected to pressurizing under the pressure of 50, 100, 250, 500, 750, 1000 and 2000 MPa for 1 h. The physical properties of pressurized starch, such as morphology, surface and crystalline structure, gelatinization parameters, were studied by means of scanning and atomic force microscopy (SEM/AFM), X-ray diffraction (X-ray), differential scanning calorimetry (DSC). The susceptibility to the amylolytic enzyme (α-amylase) was also measured. Application of pressure in the range of 50–2000 MPa results in an increase in the compressed potato starch bulk density, change in the contours of the granules from oval to polyhedral, increase in the roughness of the granule surface, vanishing of the X-ray reflexes generated by the orthogonal structure and weakening of the reflexes generated by the hexagonal structure, lowering of the enthalpy of starch gelatinization, and the enhancement of hydrolytic susceptibility of starch granules to the amylolytic enzyme.


2008 ◽  
Vol 55-57 ◽  
pp. 837-840 ◽  
Author(s):  
N. Thongmee ◽  
Anucha Watcharapasorn ◽  
Sukanda Jiansirisomboon

This study investigated fundamental of phase formation, crystal structure and calcination process for bismuth dysprosium titanate (Bi4-xDyxTi3O12; BDT) powders when x = 0, 0.25, 0.5, 0.75 and 1.0. BDT powders were prepared using a simple solid-state reaction on mixtures of reagent grade Bi2O3, Dy2O3 and TiO2 powders. The mixtures were calcined at temperature in the range of 500-800°C for 4 h at a heating/cooling rate of 5°C/min. Thermal characteristics of powders were studied using thermogravimetric/differential thermal analyses which indicated that the formation of Bi4Ti3O12 and Bi3Dy1Ti3O12 powders occurred at ~500oC. Effect of Dy3+ concentration on phase and crystal structure was investigated using X-ray diffractometry. The results revealed that at small concentration of Dy dopant (x £ 0.25), optimum calcination temperature for providing bismuth titanate-based phase was 650oC. Increasing content of Dy dopant seemed to reduce calcination temperature to 600oC. This study suggested the alternative environmental friendly BDT materials which may be used as starting powders for production of high quality BDT ceramics.


Clay Minerals ◽  
1970 ◽  
Vol 8 (3) ◽  
pp. 255-266 ◽  
Author(s):  
M. V. Eirish ◽  
L. I. Tret'Yakova

AbstractThe influence of sorbed cations and hydration on the a and b dimensions of montmorillonite, has been established by the selected area diffraction technique (S.A.D.) and by X-ray diffraction analysis. Concepts on the bonds and interaction mechanism of aluminosilicate layers with sorbed cations and water molecules (which form hydrate-ionic layers) are discussed. These concepts also indicate the basic stages of the sorption process and the formation of the montmorillonite structure. Assuming that aluminosilicate and hydrate-ionic layers represent a single crystal-chemical structure, the change of configuration of the aluminosilicate layers and dimensions of the montmorillonite lattice are explained.


Author(s):  
H.-J. Cantow ◽  
H. Hillebrecht ◽  
S. Magonov ◽  
H. W. Rotter ◽  
G. Thiele

From X-ray analysis, the conclusions are drawn from averaged molecular informations. Thus, limitations are caused when analyzing systems whose symmetry is reduced due to interatomic interactions. In contrast, scanning tunneling microscopy (STM) directly images atomic scale surface electron density distribution, with a resolution up to fractions of Angstrom units. The crucial point is the correlation between the electron density distribution and the localization of individual atoms, which is reasonable in many cases. Thus, the use of STM images for crystal structure determination may be permitted. We tried to apply RuCl3 - a layered material with semiconductive properties - for such STM studies. From the X-ray analysis it has been assumed that α-form of this compound crystallizes in the monoclinic space group C2/m (AICI3 type). The chlorine atoms form an almost undistorted cubic closed package while Ru occupies 2/3 of the octahedral holes in every second layer building up a plane hexagon net (graphite net). Idealizing the arrangement of the chlorines a hexagonal symmetry would be expected. X-ray structure determination of isotypic compounds e.g. IrBr3 leads only to averaged positions of the metal atoms as there exist extended stacking faults of the metal layers.


Planta Medica ◽  
2008 ◽  
Vol 74 (03) ◽  
Author(s):  
W Gul ◽  
P Carvalho ◽  
D Slade ◽  
M Avery ◽  
JR Duchek ◽  
...  
Keyword(s):  

Author(s):  
Süheyla Özbey ◽  
F. B. Kaynak ◽  
M. Toğrul ◽  
N. Demirel ◽  
H. Hoşgören

AbstractA new type of inclusion complex, S(–)-1 phenyl ethyl ammonium percholorate complex of R-(–)-2-ethyl - N - benzyl - 4, 7, 10, 13 - tetraoxa -1- azacyclopentadecane, has been prepared and studied by NMR, IR and single crystal X-ray diffraction techniques. The compound crystallizes in space group


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