摘要
Abstract
To establish accurate and efficient quality control standards for the purity of 1,3,5-trichloro-2,4,6-trinitrobenzene(TCTNB),the comprehensive performance of the classical acid-base titration method and a newly developed green liquid chro-matography method was systematically compared.The acid-base titration method quantifies TCTNB by hydrolyzing it with sodi-um hydroxide followed by back-titration of the excess base.The liquid chromatography method innovatively employed low-toxicity methanol instead of traditional toxic solvents and achieved baseline separation of the target compound from impuri-ties on a C18 column.Experimental results indicated that the titration method was cumbersome(requiring 5.9 hours per analy-sis)and exhibited significant inaccuracy,showing a mean measured value of 93.89%with a substantial systematic negative bias of-6.05%compared to the sample's nominal value.In contrast,the liquid chromatography method demonstrated higher effi-ciency(requiring 3.2 hours per analysis),good precision(with a relative standard deviation<0.30%,n=6),and excellent accu-racy,showing a mean value of 99.82%that closely matched the nominal value of 99.94%.The substantial systematic error in the titration method was primarily attributed to the deep color of the hydrolyzed solution,which introduced subjectivity in end-point determination,and potentially incomplete hydrolysis or interfering side reactions.The liquid chromatography method effec-tively overcame these limitations due to its superior separation selectivity and detection stability.The newly established liquid chromatography method significantly outperforms the traditional titration method in terms of accuracy,precision,efficiency,and green safety.关键词
1,3,5-三氯-2,4,6-三硝基苯(TCTNB)/液相色谱法/酸碱滴定法/纯度分析Key words
1,3,5-trichloro-2,4,6-trinitrobenzene(TCTNB)/liquid chromatography/titration/purity analysis分类
武器工业
