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AC impedance and microstructure of rye starch exposed to water vapour

Starzyk F., Chrzanowska A., Łużny W., Śniechowski M.

Archives of Materials Science and Engineering

2009

Vol. 40, nr 1

23-26

Purpose: The purpose of this paper was to record and analyse mass (m) changes of population of micro-granules of rye starch, effective alternative current (AC), (electric) complex impedance (EACI) of this system taking place during humidification as well as insight into microstructure evolution by X-ray diffraction (XRD). Design/methodology/approach: Mass changes of biopolymeric micro-granular sample occurring during its exposition to saturated water vapour at room temperature, was recorded in time by means of precise torsional balance equipped with special chamber. The same was done in case of microstructure by XRD method. Monitoring of EACI was performed by means of interdigit comb capacitor and precise RLC meter equipped with PC software. Specially designed and constructed measuring chamber was applied to control temperature and relative humidity (RH %) in ambient sample atmosphere. Electric measurements were carried out for 5 selected frequencies. Findings: Interdigit dielectric spectroscopy method turned out to be more sensitive technique to follow details of long lasting humidification than only mass changes recording. Correlation of changes of EACI with simultaneously occurring mass increase can be a way to describe the humidification stages processes involving water molecules adsorption and absorption by micro-granular biopolymeric sample. Frequency dependence of EACI gives insight into mechanism of water molecules inclusion, binding and immobilization on the starch granules surface as well as inside of its internal physical structure. Research limitations/implications: The recording duration of m(t) was limited to &sim104 s in case of humidification by balance resolution and character of the process. The whole range of measurements was limited to max &sim23 RH % of water uptake in order to prevent over molecular structure irreversible changes. The above limitations enable us to collect data for modelling reversible water uptake and connected EACI micro-granular biopolymeric population sample. Practical implications: EACI monitoring of humidification turned out to be much more selective than only gravitational measurement of mass change. Modelling purpose correlation of both can give new possibilities to modelling approach. Achieved data can contribute to better understanding of active adsorption and absorption centres in starch granules. Originality/value: For the first time practically important humidification process was monitored in statu nascendi, without disturbing geometry of starch granules population by means of EACI evolution record. It was enabled by application of interdigit comb capacitor as a sensing unit. This is the first report of four stages for EACI evolution as well as the first XRD direct record of granular starch reversal swelling.

Physicochemical changes in epoxy-amine systems studied by ionic conductivity and ionic carriers mobility measurements

Friedrich K., Ulański J., Boiteux G., Seytre G.

Polimery

2006

T. 51, nr 9

648-655

The main objective of this work was to find the correlations between the ionic conductivity, viscosity and physicochemical changes occurring during the isothermal cure of the epoxy-amine systems. The studies of the ionic conductivity evolutions have been performed using dielectric and direct-current techniques. The measurement data were compared with the ion mobility values evaluated from the time-of-flight investigations and with the dynamic viscosity determined by dynamic mechanical analysis. Different epoxy-amine reacting systems have been analyzed: the diglycidyl ether of bisphenol A with diamino-4,4'-dimethyl-3,3'-dimethyldicyclohexylmethane (DGEBA-3DCM) which gelates and vitrifies during the cure and the diglycidyl ether of 1,4-butanediol with 4,9-dioxa-1,12-dodecane diamine (DGEBD-4D) which only gelates during its polycondensation. It was found that even with an appearing of gelation or viscoelastic properties the conduction process could be described as thermally activated. The inconsistencies between ionic conductivity and ion mobility evolutions indicate that the concentration of the mobile charge carriers in the medium changes during the reaction. It was also observed that the vitrification could be responsible for the large changes of free volume in the system influencing the ionic conduction mechanism and therefore the ionic conductivity evolutions. It was also found that the Stokes's law is fulfilled at the beginning of the cure only.

Głównym celem tej pracy było znalezienie korelacji pomiędzy przewodnictwem jonowym, lepkością oraz zmianami fizykochemicznymi pojawiającymi się podczas izotermicznego utwardzania układów epoksydowo-aminowych. Badania zmian przewodnictwa jonowego dokonane zostały przy użyciu technik dielektrycznych i stałoprądowych (rys. 2-6). Następnie wyniki pomiarów porównano z wartościami ruchliwości jonów oszacowanymi z badań czasu przelotu jonów metodą time-of-flight (TOF) oraz z wartościami lepkości dynamicznej określonymi metodą dynamicznej analizy mechanicznej (DMA) (rys. 7). Analizowano różne układy reaktywne epoksydowo-aminowe: eter diglicydowy bisfenolu A z diamino-4,4'-dimetylo-3,3'-dimetylodicyklohexylometanem (DGEBA-3DCM), który żeluje i ulega zeszkleniu podczas procesu utwardzania oraz eter diglicydylowy 1,4-butanodiolu z 4,9-dioksa-1,12-dodekano diaminy (DGEBD-4D), który podczas polikondensacji wyłącznie żeluje (tabela 2). Stwierdzono, że nawet w przypadku pojawienia się żelowania lub właściwości elastycznych proces przewodzenia może być opisany jako aktywowany termicznie. Niezgodności pomiędzy zmianami przewodnictwa jonowego i ruchliwości jonów wskazują, że w procesie utwardzania następują zmiany koncentracji ruchliwych jonów. Wykazano, że prawo Stokesa może być spełnione wyłącznie na początku procesu utwardzania.