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61.
62.
The effects of temperature and duration of melting on the rate of isothermal crystallization of isotactic polypropylene were investigated by differential scanning calorimetry (DSC). Crystallization rates were found to decrease with increasing melt temperature and melting time. The results were discussed in the framework of the theoretical model of transient isothermal crystallization developed by the present authors [1]. The results suggest gradual destruction of predetermined nuclei with activation energyE
a=89±7 kJ/mole as a main mechanism of the observed effects.This work and Part I of this research [1] have been supported in part by Research Grant Number PB 1291/52/93/04 from State Committee for Scientific Research (KBN), Poland, and by 40% MURST founds, Italy. 相似文献
63.
The thermodynamic model of inorganic arsenic was validated by comparing the predicted As(III) concentration with the experimentally determined one in several river waters samples of the Basque Country (Spain) collected in two sampling campaigns: spring and autumn 2000. This model takes into account the acid-base equilibria of As(III) and As(V) together with the redox equilibria between the H3AsO3 and H3AsO4 species. A correct prediction of As(III) concentration requires the knowledge of the total concentration of arsenic, pH, redox potential (referred to hydrogen electrode), and ionic strength values of the solution. The estimation of the activity coefficients of the arsenic species was performed by means of the Modified Bromley’s Methodology (MBM).In order to perform the experimental As(III) determination, an analytical method was implemented by using an ion exchange separation of As(III)/As(V) on a continuous FIA-IE-HG-AAS system. The total arsenic concentration was determined together with total concentration of the main alkaline or alkaline-earth metals and anions in the natural waters. Temperature compensated measurements of the pH and redox potentials were made in-situ at the sampling sites.For both seasonal campaigns, the agreement between predicted and experimental As(III) is really high for those samples belonging to non polluted river waters. 相似文献
64.
There is a need to develop reliable portable analytical systems for on-site and real-time biomonitoring of lead (Pb) from both occupational and environmental exposures. Saliva is an appealing matrix since it is easily obtainable, and therefore a potential substitute for blood due to existing reasonably good correlation between Pb levels in blood and saliva. The microanalytical system is based on flow-injection/stripping voltammetry with a wall-jet (flow-onto) microelectrochemical cell. Samples that contain as little as 1% saliva can cause electrode fouling, resulting in significantly reduced responsiveness and irreproducible quantitations. In addition, incomplete Pb release from salivary protein can also yield a lower Pb response than expected. This paper evaluates the extent of in vitro Pb-protein binding and the optimal pretreatment for releasing Pb from the saliva samples. Even in 50% by volume of rat saliva, the electrode fouling was not observed, due to the appropriate sample pretreatment and the constant flow of the sample and acidic carrier that prevented passivation by the protein. The system offered a linear response over a low Pb range of 1-10 ppb, low detection limit of 1 ppb, excellent reproducibility, and reliability. It also yielded the same Pb concentrations in unknown samples as did the ICP-MS. These encouraging results suggest that the microanalytical system represents an important analytical advancement for real-time non-invasive biomonitoring of Pb. 相似文献
65.
Paraskevas D. Tzanavaras Demetrius G. Themelis Anastasios Economou Georgios Theodoridis 《Mikrochimica acta》2003,142(1-2):55-62
Two new simple and rapid methods are reported for the accurate and precise spectrophotometric determination of captopril
(CPL) using flow (FI) and sequential injection (SI) analysis. The methods are based on the fast oxidation of CPL by Fe(III).
The produced Fe(II) reacts with 2,2′-dipyridyl-2-pyridylhydrazone (DPPH) in acidic medium to form a colored complex which
is monitored spectrophotometrically at 535 nm. Both methods allow the determination of the analyte up to 1000 mg L−1 at a sampling rate of 120 and 60 injections per hour for FI and SI, respectively. The methods are very precise [s
r=0.8 and 1.2% at 500 mg L−1 CPL (n=12) for FI and SI, respectively] and the 3σ detection limits (c
L=4.0 and 7.0 mg L1, respectively) are quite satisfactory. Their application to a variety of anti-hypertensive commercial pharmaceutical formulations
showed excellent results (relative errors, e
r, < ± 1.6% in all cases compared to an official HPLC method), while common pharmaceutical excipients were found not to interfere.
Recovery experiments further verified the accuracy of the developed methods, as the percent recoveries were in the range of
98.1–102.5%.
Author for correspondence. E-mail: themelis@chem.auth.gr
Received May 9, 2002; accepted January 8, 2003
Published online May 5, 2003 相似文献
66.
CE conditions for monitoring the unsaturated disaccharides of hyaluronic acid (di-HA) and chondroitin sulfate (di-CS) using an alkaline tetraborate buffer, electrokinetic sample injection, and UV absorption detection at 232 nm are reported. Separations were performed in an uncoated fused-silica capillary having reversed polarity and reversed electroosmosis generated with the addition of CTAB to the buffer. The influence of various separation parameters, including the concentration of CTAB, buffer pH, concentration of tetraborate, and applied voltage, on the resolution of the two disaccharides was investigated. Baseline separation was obtained with 25 mM tetraborate at pH 10.0 and having 0.05 mM CTAB. Chloride and phosphate in the sample are beneficial for the stacking of the disaccharides, with di-HA forming a much sharper peak than di-CS. Using samples prepared in 25 mM Tris-HCl (pH 7.5) and electrokinetic injection at the cathode at -10 kV for 40 s, linear relationships between the corrected peak area and the concentration of the disaccharides have been found in the ranges of 1.0-400.0 and 0.1-1.0 microg/mL (0.2-1.0 microg/mL for di-CS), with correlation coefficients being >0.9933 in all cases. The RSDs of detection times and corrected peak areas were between 1.13-1.24 and 1.57-2.13%, respectively. Applied to human serum samples that were prepared by ethanol precipitation and depolymerization of the two polysaccharides with chondroitinase ABC reveals comigration of endogenous compounds with di-HA and a sample-dependent detection time. The di-HA content in the serum sample can be estimated via subtraction of the blank peak that is obtained without enzymatic hydrolysis. 相似文献
67.
Determination of Gossypol in Trace Level by Flow Injection Analysis with Chemiluminescence Detection
Bing Chun XUE Er Bao LIU College of Chemistry Life Sciences Tianjin Normal University Tianjin 《中国化学快报》2006,17(1):57-60
Gossypol, [1, 1′, 6, 6′, 7,7′-hexahydroxyl-5,5′-diisopropyl-3,3′-dimethyl-(2,2′-binaphtha- lene)-8,8′-dicarboxaldehyde] is a polyphenolic yellow compound naturally occurring in various parts of cotton plants1. The compound has been associated with 相似文献
68.
69.
Bernhard Wunderlich 《Thermochimica Acta》2003,403(1):1-13
Linear, flexible macromolecules are long recognized as phase structures limited to micrometer and nanometer dimensions with covalent bonds crossing the interfaces. This special, usually non-equilibrium structure leads to unique properties and a multitude of changes for different thermal and mechanical histories. Analyses that enable the study of these properties are temperature-modulated calorimetry and related techniques which allow the separation of equilibrium and non-equilibrium responses. Research on these topics is reviewed and combined to a model for the nanophases. The new approach to the complex nanophase systems yields a better understanding of the relationship between structure and thermodynamic properties. Special emphasis is placed on the size and surface effects on the glass and melting transitions, the development of rigid-amorphous phases, and the reversible melting within the globally metastable structure. 相似文献
70.
流动注射分光光度法测定微量铜的研究 总被引:5,自引:0,他引:5
研究了在TritonN-101存在下,2-羟基-3-羧基-5-磺酸基苯重氮氨基偶氮苯(HCS-DAA)显色流动注射光度测定微量铜的新方法,用pH0.4~11.5Na2B4O7-NaOH缓冲溶液作载流,HCSDAA和TritonN-101的混合试剂作试剂流,采双道流路,530nm检测反应生成红色配合物,方法线性范围是0.024~0.20μg/mL,检出限为8ng/mL,进样频率为100样次/h,直接 相似文献