Department of Chemistry and Chemical Biology of Rutgers, The State University of New Jersey, New Jersey Center for Biomaterials, Piscataway, NJ 08854, United States.
Talanta. 2009 Nov 15;80(1):231-5. doi: 10.1016/j.talanta.2009.06.059. Epub 2009 Jul 4.
Methods for the detection and estimation of diphosgene and triphosgene are described. These compounds are widely used phosgene precursors which produce an intensely colored purple pentamethine oxonol dye when reacted with 1,3-dimethylbarbituric acid (DBA) and pyridine (or a pyridine derivative). Two quantitative methods are described, based on either UV absorbance or fluorescence of the oxonol dye. Detection limits are approximately 4 micromol/L by UV and <0.4 micromol/L by fluorescence. The third method is a test strip for the simple and rapid detection and semi-quantitative estimation of diphosgene and triphosgene, using a filter paper embedded with dimethylbarbituric acid and poly(4-vinylpyridine). Addition of a test solution to the paper causes a color change from white to light blue at low concentrations and to pink at higher concentrations of triphosgene. The test strip is useful for quick on-site detection of triphosgene and diphosgene in reaction mixtures. The test is easy to perform and provides clear signal readouts indicative of the presence of phosgene precursors. The utility of this method was demonstrated by the qualitative determination of residual triphosgene during the production of poly(bisphenol-A carbonate).
描述了二氯甲醚和三氯甲醚的检测和估算方法。这些化合物是广泛使用的光气前体，当与 1,3-二甲基巴比妥酸 (DBA) 和吡啶（或吡啶衍生物）反应时，会产生强烈着色的紫色五甲川菁氧杂萘染料。描述了两种定量方法，一种基于 oxonol 染料的紫外吸收，另一种基于荧光。紫外检测的检出限约为 4 微摩尔/升，荧光检测的检出限<0.4 微摩尔/升。第三种方法是一种检测二氯甲醚和三氯甲醚的简单快速检测和半定量估计的试条，使用嵌入二甲巴比妥酸和聚（4-乙烯基吡啶）的滤纸。将测试溶液添加到滤纸上会导致颜色从白色变为低浓度的浅蓝色，再变为较高浓度的三氯甲醚的粉红色。该试条可用于快速现场检测反应混合物中的三氯甲醚和二氯甲醚。该测试易于进行，并提供清晰的信号读数，表明存在光气前体。该方法的实用性通过在生产聚（双酚 A 碳酸酯）期间定性测定残留的三氯甲醚得到了证明。
