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111.
Crystallization behaviour of blends of poly(N-methyldodecano-12-lactam) (PMDL) with statistical copolymer poly(styrene-stat-acrylic acid) (PSAA) has been studied by the DSC and WAXD methods. The blend films prepared from dioxane solutions were crystallized at laboratory temperature for five days. Approximate crystallinities of as-prepared neat lower- PMDL 5 and higher-molecular weight PMDL 45 were 28% and 19%, respectively. With increasing PSAA content in the blends the crystallinities decreased sharply. The melting point of the primary crystalline structure of PMDL showed a decreasing dependence on PSAA content in the blends, confirming miscibility of the PMDL-PSAA pair. Recrystallization was strongly suppressed in the blends. The lower-melting endotherm appearing at about 10-15 °C above the crystallization temperature was attributed to melting to less perfect structures formed during secondary crystallization. In neat PMDL, the extent of secondary crystallization was approximately 5-10%. In the blends containing 20% PSAA approximate relative proportion of secondary crystallites on total crystallinity was 40% and 60% for the blends with PMDL 5 and PMDL 45, respectively. WAXD measurements did not reveal any change in crystal modification on blending. Increased Tg in blends of flexible PMDL cannot play a significant role in suppression of primary in favour of secondary crystallization. This was attributed to low mobility of PMDL chains due to dilution effect and specific interactions with the amorphous copolymer component, and, in case of the higher-molecular-weight PMDL, a greater involvement of entanglements. Higher Tg of blends was involved in retardation of non-isothermal crystallization on cooling and subsequent cold crystallization.  相似文献   
112.
The preconcentration and voltammetric behavior of BiIII on a sodium humate modified carbon paste electrode was studied by means of cyclic voltammetry (CV) and differential pulse stripping voltammetry (DPSV). The proposed measurement involves an initial nonelectrolytic preconcentration step in which BiIII is complexed by the surface modifier in a solution of 0.05 M KNO3-0.0106 M HNO3 (pH 2.0) and a subsequent electrochemical scan step in which the preconcentrated BiIII was reduced and then oxidized promptly in supporting electrolyte of 0.5 M HNO3. The resulting DPSV anodic current was proportional to the concentration of BiIII ion over the range of 4.78 × 10−8–1.44 × 10−5 M. The detection limit was 4.78 × 10−8 M. The proposed method was used to determine bismuth in various samples. Various factors affecting the electrode behavior were also investigated at the same time.  相似文献   
113.
速差动力学分析及其应用进展   总被引:9,自引:2,他引:9  
方国桢  郭忠先 《分析化学》1993,21(11):1347-1354
速差动力学分析是不经分离同时或连续测定混合物中性质密切相关的多组份的重要方法。本文综述了该法在1989-1992年间国内外新进展,尤着重其在有机,生物混合物中多组份分析的应用及新的计算方法,化学计量学的引入。引用最新文献67篇。  相似文献   
114.
The blends of poly(N-methyldodecano-12-lactam) (MPA) with poly(styrene-co-acrylic acid) (PSAA) prepared from dioxane solutions were studied by differential scanning calorimetry (DSC) and Fourier transform infrared spectroscopy (FTIR). The experimental DSC data of glass transition temperature Tg as a function of composition of amorphous phase were fitted for the as-prepared and re-scanned samples using theoretical approaches. The as-prepared blends show monotonic single-Tg dependence. The values of the Gordon-Taylor coefficient not far from unity suggest miscibility of the blend system in amorphous phase in the whole concentration range. As documented by FTIR, this miscibility is associated with hydrogen bonds between COOH groups of the acrylic acid units in PSAA molecules acting as the H-bond donor and CO groups of MPA acting as the H-bond acceptor. The Tg-dependencies obtained form the second runs have a profound sigmoid character. The Schneider treatment induced an idea of partial limited miscibility in the MPA/PSAA blends caused by prevalence of homogeneous contacts. The difference in Tg between the first and second run can partly be attributed to higher crystallinities in the former.  相似文献   
115.
This review critically evaluates the plastic accumulation challenges and their environmental (primarily) and human (secondarily) impacts. It also emphasizes on their degradation and fragmentation phenomena under marine conditions. In addition, it takes into account the leachability of the various chemical substances (additives) embedded in plastic products to improve their polymeric properties and extend their life. Regardless of their effectiveness in enhancing the polymeric function of plastic products, these additives can potentially contaminate air, soil, food, and water. Several findings have shown that, regardless of their types and sizes, plastics can be degraded and/or fragmented under marine conditions. Therefore, the estimation of fragmentation and degradation rates via a reliable developed model is required to better understand the marine environmental status. The main parameter, which is responsible for initiating the fragmentation of plastics, is sunlight/UV radiation. Yet, UV- radiation alone is not enough to fragment some plastic polymer types under marine conditions, additional factors are needed such as mechanical abrasion. It should be also mentioned that most current studies on plastic degradation and fragmentation centered on the primary stages of degradation. Thus, further studies are needed to better understand these phenomena and to identify their fate and environmental effects.  相似文献   
116.
Robert Piech 《Talanta》2007,72(2):762-767
Hanging copper amalgam drop electrode has been applied for trace determination of arsenic by cathodic stripping analysis. Detection limit for As(III) as low as 0.33 nM (0.02 μg/L) at deposition time (240 s) could be obtained. For seven successive determinations of As(III) at concentration of 5 nM relative standard deviation was 2.5% (n = 7). Interferences from selected metals and surfactant substances were examined. Absence of copper ions in sample solution causes easier optimization and makes method less vulnerable on contamination. The developed method was validated by analysis of certified reference materials (CRMs) and applied to arsenic determinations in natural water samples.  相似文献   
117.
Zusammenfassung Aus dem Maximalwert einer Differentialthermoanalysenkurve kann die Temperatur einer Phasenumwandlung abgeleitet werden. Für die Auswertung benötigt man Kurven, die bei verschiedener Aufheizgeschwindigkeit gemessen wurden. Das Verfahren wurde an K2SO4 und BaCO3 getestet. Die Experimente ergaben 583,3 bzw. 809,6°C.Herrn Prof. Dr. H. Hausner danke ich für die Förderung dieser Arbeit und Frau H. Tyrlas für die umsichtige und sorgfältige Durchführung der Experimente.  相似文献   
118.
The polarographic behaviour of 2-nitronaphthalene was investigated by DC tast polarography (DCTP) and differential pulse polarography (DPP), both at a dropping mercury electrode, and differential pulse voltammetry and adsorptive stripping voltammetry, both at a hanging mercury drop electrode. Optimum conditions have been found for the determination of 2-nitronaphthalene by the given methods in the concentration ranges of 2×10–6–1×10–4, 2×10–7–1×10–4, 1×10–8–1×10–4 and 2×10–9–1×10–8 M, respectively. Practical applicability of these techniques was demonstrated by the determination of 2-nitronaphthalene in drinking and river water after its preliminary separation and preconcentration using liquid–liquid and solid-phase extraction with limits of determination of 3×10–10 M (drinking water) and 3×10–9 M (river water).  相似文献   
119.
《Electroanalysis》2006,18(2):127-130
The voltammetric behavior of 2‐methyl‐4,6‐dinitrophenol was investigated by differential pulse voltammetry (DPV) at a nontoxic mercury meniscus‐modified silver solid amalgam electrode (m‐AgSAE). Conditions have been found for its determination by DPV at m‐AgSAE in the concentration range of 0.2 to 1 μmol L?1.  相似文献   
120.
A modified electrode is fabricated by embedding gold nanoparticles into a layer of electroactive polymer, poly(4-aminothiophenol) (PAT) on the surface of glassy carbon (GC) electrode. Cyclic voltammetry (CV) is performed to deposit PAT and concomitantly deposit Au nanoparticles. Field emission transmission electron microscopic image of the modified electrode, PAT-Aunano-ME, indicates the presence of uniformly distributed Au nanoparticles having the sizes of 8-10 nm. Electrochemical behavior of the PAT-Aunano-ME towards detection of ascorbic acid (AA) and dopamine (DA) is studied using CV. Electrocatalytic determination of DA in the presence of fixed concentration of AA and vice versa, are studied using differential pulse voltammetry (DPV). PAT-Aunano-ME exhibits two well defined anodic peaks at the potential of 75 and 400 mV for the oxidation of AA and DA, respectively with a potential difference of 325 mV. Further, the simultaneous determination of AA and DA is studied by varying the concentration of AA and DA. PAT-Aunano-ME exhibits selectivity and sensitivity for the simultaneous determination of AA and DA without fouling by the oxidation products of AA or DA. PAT and Au nanoparticles provide synergic influence on the accurate electrochemical determination of AA or DA from a mixture having any one of the component (AA or DA) in excess. The practical analytical utilities of the PAT-Aunano-ME are demonstrated by the determination of DA and AA in dopamine hydrochloride injection and human blood serum samples.  相似文献   
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