碱解增敏荧光法测定残留甲萘威

甲萘威在0.01mo1/L KOH溶液中可降解为强荧光产物。十六烷基三甲基溴化铵对其增敏后,荧光强度达到其自身荧光强度的6倍。基于此,建立了对残留甲萘威进行荧光测定的新方法。线性动态范围为2.00~1.70×103μg/L;检出限为0.95μg/L;样品的加标回收率在90.2%~99.9%。本法成功地用于叶菜中残留甲萘威的测定。     

高温燃烧水解-离子色谱法测定煤中的氟和氯

建立高温燃烧水解-离子色谱法测定煤中氟和氯含量的方法。间隔测量煤标准物质和待测煤样,以煤标准物质特性量值的变化扣除系统漂移的影响,提高了测定结果的准确度和重复性。氟含量在0.042~2.018μg/mL范围内与其色谱峰面积呈良好的线性关系,线性相关系数r=0.995 8,检出限为0.011μg/g,测量结果相对标准偏差为6.32%(n=6);氯含量在0.046~2.292μg/mL范围内与其色谱峰面积呈良好的线性关系,线性相关系数r=0.999 8,检出限为0.010μg/g,测量结果的相对标准偏差为0.7%(n=6)。用该方法对煤标准物质进行测定,氟、氯测定结果与标准值一致。该方法简便快速,灵敏度高,结果准确,可用于煤中氟和氯含量的测定。     

猪毛水解母液中氨基酸的反相高效液相色谱分析

A new method for separation and quantification of amino acids by pre-column derivatization withphenylisothiocyanate(PITC ) and reversed-phase HPLC is described. Seventeen amino acids were separatedin 30 min at room temperature.The method has been successfully applied to the determination of amino acidcomposition in the solution which was prepared by hydrolyzing pig hair and extration of cystine.     

Preparation of halogen-free flame retardant polyacrylonitrile via hydrolyzing and grafting with diphenylphosphinyl chloride

Abstract

Halogen-free flame retardant polyacrylonitrile (PAN) was prepared via hydrolyzing the nitrile groups of PAN using aqueous sodium carbonate solution/hydrogen peroxide followed by grafting with diphenylphosphinyl chloride. The structure of original PAN, hydrolyzed PAN (HPAN), and flame retardant PAN (FR-PAN) samples were characterized using Fourier transform infrared spectroscopy, X-ray photoelectron spectroscopy, X-ray diffraction, and ¹H NMR spectroscopy. The thermal properties of the materials were assessed using thermogravimetric analysis. The FTIR spectroscopy indicates that a carbonyl group is present in hydrolyzed HPAN and some characteristic PAN absorption peaks decreased slightly upon hydrolysis. The XPS results show that FR-PAN contained phosphorus, indicating that diphenylphosphinyl chloride has been grafted onto HPAN, which is in accordance with the phenomenon of the self-extinguishing phenomena of FR-PAN during burning experiments. The TG curves indicate the presence of a char residue for FR-PAN of 45% at 800?°C, a higher char residue than that of original PAN (39%). Therefore, FR-PAN displays better thermal stability and char forming capability than does the untreated polymer.