比色法测定声表面波化学传感器膜材料(SXFA)的叔羟基
Colorimetric Determination of Tertiary Hydroxyl Group in the Membrane Material (SXFA) of SAW Chemosensor
摘 要
聚[甲基(4-羟基-4,4-双-三氟代甲基)-丁-1-烯基]-硅氧烷(SXFA)样品中的叔羟基与氢碘酸反应生成三烷基碘化物,在pH 4的硫酸(1+9)溶液中,所得三烷基碘化物与碘酸钾作用定量生成碘单质,含碘的环己烷溶液在525nm波长有吸收,据此提出了比色法测定声表面波传感器膜材料SXFA的叔羟基的方法.以叔丁醇为标准样品,以其羟基的质量为横坐标,吸光度为纵坐标,绘制标准工作曲线,将SXFA的吸光度代入工作曲线,由此计算得SXFA中叔羟基的含量.将样品在氧气瓶中燃烧,用水吸收生成的氟化氢气体,用离子色谱仪测定了SXFA中氟元素的含量.结果表明,所得氟与叔羟基的物质的量的比与结构式相符.
叔羟基
定量分析
离子色谱法
Colorimetry
Tertiary hydroxyl group
Quantitative analysis
Ion chromatography
Abstract
The trialkyliodide was formed by the reaction of tertiary hydroxyl group in SXFA with HI. In H2SO4 solution (1+9) of pH 4,I2 was generated quantitatively by the reaction of trialkyliodide with KIO3,and the I2 was dissolved in cyclohexane,having its absorption maximum at 525nm. Based on these factors,the determination of tertiary hydroxyl group in SXFA by colorimetry was proposed. Tert-butyl alcohol was used as standard sample for preparation of standard curve,taking the mass of hydroxyl group as the ordinate and values of absorbance as the abscissa. The content of hydroxyl group in SXFA was found from the standard curve with the values of the absorbance measured. The sample was burned in oxygen bomb,HF gas obtained was absorbed with water,and the content of F in SXFA was determined by ion chromatograph. It was found that the molar ratio of F to hydroxyl group obtained was checked quite well with that in the structural formula.
中图分类号 O657
所属栏目 工作简报
基金项目
收稿日期 2009/1/19
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备注王超宇(1972-),男,黑龙江人,硕士,研究方向为功能高分子.
引用该论文: WANG Chao-yu. Colorimetric Determination of Tertiary Hydroxyl Group in the Membrane Material (SXFA) of SAW Chemosensor[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2009, 45(7): 847～848
王超宇. 比色法测定声表面波化学传感器膜材料(SXFA)的叔羟基[J]. 理化检验－化学分册, 2009, 45(7): 847～848
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参考文献
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【2】NOVAK P,ILAVSKY M,PAVALS P,et al. The problem of determination of hydroxyl groups in poly(oxyethylene) diols by using the phenyliso-cyanate method[J]. Die Angerw Makromol Chem,1990,179:87-98．
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【4】吴美玉,雍忠根,金一.F-NMR法测定聚醚多元醇中伯羟基的相对含量[J].高分子学报,1988(2):149-151．
【5】FLOYD F-LHO. Characterization and quantitative measurement of hydroxyl groups in polymers by fluorine-19 NMR of hexafluoroacetone adducts[J]. Analytical Chemistry,1973,45(3):603-605．
【6】董云,张琪.用动态酰化法测定聚醚中的伯羟基[J].江苏化工,1981(3):62-64,80．
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