TGA analysis of γ‐irradiated linear low‐density polyethylene

Linear low‐density polyethylene (LLDPE), based on butene‐1 or hexene‐1, was irradiated with γ‐rays under vacuum or in the presence of air. The study focused on the influence of the dose rate and the γ‐dose on the thermal properties of LLDPE. Differential scanning calorimetry, thermogravimetric analysis (TGA), and TGA/FTIR techniques were used to address the thermal behavior as a result of γ‐irradiation. During this irradiation, competition between crosslinking and scission reactions, subsequent to oxidation reactions, occurred in the polymeric material, which strongly depends on the experimental conditions. A decrease of the crystallinity for γ‐irradiated samples was observed in particular for samples irradiated under vacuum. This observation may be explained by increased hindrance of segment mobility due to crosslinking reactions that prevent crystal growth. TGA investigations revealed an enhancement of the thermal stability for samples irradiated under vacuum but not for those irradiated in air. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 100: 2790–2795, 2006     

The crystallization characterization of bulk syndiotactic polystyrene sample: immediate evidence from IR spectroscopy

The crystallization characterization of bulk syndiothactic polystyrene (s-PS) sample is thoroughly studied using the Fourier transform infrared spectroscopy (FTIR). The WAXD is further used to identify the s-PS crystal formation to confirm the specific absorbance in FTIR spectra. Both melt and cold-crystallization behavior are quantitatively determined using FTIR spectra ranging from 870 to 820 cm⁻¹ at 264 °C. Fitting curves to IR spectra provides direct evidence of bulk s-PS crystallization behavior in quantification. The melt-crystallization process yields the β-form only; while the cold-crystallization process yields both the α and the β-form crystal in bulk s-PS sample. The β-form crystal is generated from the phase-transformation of the α-form crystal by cold-crystallization process, the α-form crystal is the initial phase. The activity energy of the α-form formation is lower that that of the β-form, suggesting that the α-form crystal is kinetically favorable while the β-form crystal is thermodynamically favorable.     

几种光谱方法(FTIR、FT-Raman,NMR)在橡胶分析中的应用

综述了傅里叶变换红外光谱 ,傅里叶变换拉曼光谱以及核磁共振波谱在橡胶结构的定性、定量分析中的应用     

基于循环检测的气动退化图像混合域去噪算法

气动退化图像中存在先验信息未知以及噪声成分复杂不易进行滤波处理的问题,为此,提出一种气动退化图像混合域去噪算法。设计针对高斯噪声、泊松噪声、固定值脉冲噪声和随机值脉冲噪声的混合检测方法,使用改进的滤波方法在空域去除固定值脉冲噪声和随机值脉冲噪声,进行非下采样轮廓波变换多层分解,在变换域使用阈值方法去除高斯噪声和泊松噪声。进行噪声循环检测,设定迭代停止条件控制算法循环从而实现算法自适应。仿真实验结果表明,该算法的噪声检测性能和滤波性能较好,图像细节信息得到正确恢复。同时,算法复杂度较低,实时性较好,可满足气动退化图像去噪处理的需要。     

基于图像纹理复杂度的小波域数字水印算法

针对水印信息嵌入量小、鲁棒性弱、遮蔽性差的问题,提出一种基于图像纹理复杂度的小波域人类视觉系统的水印算法。该算法将载体图像进行分块,计算每块的图像熵,并根据图像熵对载体图像的纹理特征区域进行分类,不同纹理特征水印的嵌入量不同。利用Logistic映射对水印信号进行置乱变换,将水印信号嵌入到二层离散小波变换的低频系数中,并利用小波域人类视觉模型控制水印的嵌入强度。在提取水印时,通过水印误码率和峰值信噪比评价水印质量。实验结果表明,该算法能抵抗噪声干扰、裁剪和密钥攻击,水印图像具有较强的鲁棒性和良好的遮蔽性。     

基于NSST和RI-LPQ的纹理图像检索

针对采用单一方法提取图像特征时检索率不高的问题,结合非下采样剪切波变换(NSST)统计特征和旋转不变的局部相位量化(RI-LPQ)原理,提出一种纹理图像检索方法。非下采样剪切波不仅具有方向选择性及平移不变性,而且可以对图像进行有效的稀疏表示,与传统小波相比,可有效捕捉图像的边缘轮廓等纹理信息,与非下采样轮廓波相比,具有更高的计算效率。利用广义高斯分布函数对图像NSST高频子带系数的统计特征进行分析,RI-LPQ描述算子直接提取图像特征,采用具有权重系数的相似性测度公式对Brodatz图像库进行纹理图像检索。实验结果表明,与传统小波和轮廓波的方法相比,NSST统计特征方法的平均检索率分别提高4.77%和1.44%,纹理图像检索方法的平均检索率分别提高7.36%和1.98%。     

Mode of oleic acid adsorption on rice hull ash cristobalite

Fourier transform infrared spectroscopy was used to investigate the adsorption of oleic acid (OA) onto dry rice hull ash (RHA) silica. Adsorption partially occurred by surface hydrogen bonding of the carboxylic acid. There was also formation of carboxylate ions by reaction of OA with residual potassium oxide. These ions were strongly bound by the ash. Isopropanol inhibited OA adsorption by H-bonding and encouraged desorption of H-bonded OA, but without itself being significantly bound. RHA with 40% moisture also adsorbed a small amount of OA by H-bonding and reacted with OA to form and adsorb carboxylate ions.     

Diffuse reflectance fourier transform infrared spectroscopy of phospholipid adsorption onto silicic acid

Diffuse reflectance Fourier transform infrared spectroscopy was used to study the mode of adsorption of phosphatidylcholine (PC) in hexane onto silicic acid (SA). PC adsorption was mainly through the charged phosphate group with minimal binding through the ester carbonyl. When the SA surface with adsorbed PC is washed with hexane, containing a small concentration of isopropanol, the desorbed PC is recovered without structural change, i.e., there is no evidence of PC hydrolysis in the adsorption process. Adsorbent misture probably promotes PC adsorption due to the increased availability of surface water hydroxyl groups for interaction with the PC phosphate groups. Isopropanol promoted PC binding by destabilizing PC reverse miscelles in solution, thus promoting its adsorption.     

Fatty acid composition of spanish shortenings with special emphasis on <Emphasis Type="Italic">trans</Emphasis> unsaturation content as determined by fourier transform infrared spectroscopy and gas chromatography

A Fourier transform infrared spectroscopic procedure was used to analyze 34 edible fats (22 shortenings and 12 vegetable margarines) as neat fats (IR_NF) to determine their total trans fatty acid (TFA) content. The sloping baseline was corrected with a reference spectrum based on a nonprocessed olive oil. The calibration was done using seven partially hydrogenated fats with an individual TFA content previously determined by the combination of gas chromatography (GC) with argentation thin-layer chromatography. Taking into account the different absorptivities of various trans isomers, different correction factors were calculated using the calibration standards (0.83 and 1.71 for single trans bonds in both diethylene and triethylene and for trans, trans-diethylene fatty acids, respectively) and applied to calculate the total TFA of samples. Moreover, the samples were converted to their methyl esters and reanalyzed following the same procedure (IR_FAME). Differences in TFA content of fats were not found when a t-test was used to compare the results obtained by IR_NF vs. either IR_FAME or GC, suggesting that IR of neat fats could be used, thus avoiding the need to prepare sample solutions in organic solvents and to prepare fatty acid methyl esters. The mean TFA content (determined by IR_NF) of a representative group of Spanish shortenings (22 samples) that varied widely in terms of fat sources, processes, and purposes (bakery, sandwiches, ice cream, coatings, chocolate coverings) was 6.55±11.40%, although more than 54% contained <3% of TFA. Fatty acid composition of shortenings by direct GC using a 100-m polar cyanopolysiloxane capillary column indicated that the mean trans-18∶2 isomer content was 0.58%, ranging from 0.9 to 3.4%. Small amounts of trans-18∶3 isomers (<0.3%) were observed in 18 of the 22 shortenings studied; the maximal value was <2%. The mean value of the fraction saturated+TFA of shortenings was high (59.95±12.73%), including two values higher than 83%.     

Persistence Heterogeneity Testing in Panels with Interactive Fixed Effects

We consider large N,T panel data models with fixed effects, a common factor allowing for cross‐section dependence, and persistent data and shocks, which are assumed fractionally integrated. In a basic setup, the main interest is on the fractional parameter of the idiosyncratic component, which is estimated in first differences after factor removal by projection on the cross‐section average. The pooled conditional‐sum‐of‐squares estimate is consistent but the normal asymptotic distribution might not be centred, requiring the time series dimension to grow faster than the cross‐section size for correction. We develop tests of homogeneity of dynamics, including the degree of integration, that have no trivial power under local departures from the null hypothesis of a non‐negligible fraction of cross‐section units. A simulation study shows that our estimates and tests have good performance even in moderately small panels.