Determination of trace amounts of hydroperoxides by column liquid chromatography and colorimetric detection
Determination of trace amounts of hydroperoxides by column liquid chromatography and colorimetric detection
复制标题
柱液相色谱-比色检测法测定痕量氢过氧化物
DOI：
10.1016/s0021-9673(00)93827-5
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发表时间：
1976
影响因子：
4.1
通讯作者：
J. D. V. Berg
中科院分区：
文献类型：
--
作者：
R. S. Deelder;M. Kroll;J. D. V. Berg
通过向柱流出物中连续加入合适的比色剂并连续监测反应混合物的吸光度，可以对液相色谱柱流出物中分离的化合物进行灵敏和选择性的测定。然而，在这些系统中，可能会出现相当数量的额外的色谱峰展宽，特别是如果反应较慢，需要更长的停留时间，以在reactors.It显示如何使用填充反应器，这种额外的展宽可以减少到可接受的水平。本文讨论了这类反应器的一般特点，提出了优化设计的原则，并介绍了一种测定烃类氧化反应混合物中氢过氧化物的方法。通过吸附色谱法进行分离。在在线填充反应器中，在碘化钠的酸性溶液中通过氢过氧化物形成碘，并且在362 nm处测量反应混合物的吸光度。在反应器中在70° C的温度下1.5分钟的延迟时间涉及小于1秒的停留时间分布的标准偏差。通过这种比色检测器可以测定纳克量的氢过氧化物。
The sensitive and selective determination of separated compounds in effluents from liquid chromatographic columns can be carried out by continuously adding a suitable colorimetric agent to the column effluent and continuously monitoring the absorbance of the reaction mixture. However, a considerable amount of additional broadening of the chromatographic peaks may occur in these systems, especially if slower reactions make it necessary for longer residence times to be used in the reactors.It is shown how this additional broadening can be reduced to an acceptable level by using packed reactors. Some general characteristics of these reactors are discussed and rules for the optimal design are given.A method is described for the determination of hydroperoxides in reaction mixtures from the oxidation of hydrocarbons. Separations are carried out by adsorption chromatography. In an on-line packed reactor, iodine is formed by hydroperoxides in an acidic solution of sodium iodide, and the absorbance of the reaction mixture is measured at 362 nm. A delay time of 1.5 min at a temperature of 70° in the reactor involved a standard deviation of the residence time distribution of less than 1 sec. Nanogram amounts of hydroperoxides can be determined by means of this colorimetric detector.