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升華提純法制備三氯叔丁醇高純試劑的研究

發(fā)布時間:2019-06-02 05:12
【摘要】:采用升華提純法制備半水合三氯叔丁醇高純試劑,探索了升華溫度和升華時間對工藝的影響。利用氣相色譜儀(GC)和電感耦合等離子體質(zhì)譜(ICP-MS)測試升華前后半水合三氯叔丁醇的純度和金屬離子含量的變化。參照美國西格瑪試劑指標對樣品進行檢測分析,結果表明半水合三氯叔丁醇在100℃下升華14 h,收率達98.2%,不出現(xiàn)分解,所得試劑純度高達99.96%,并具有較低的金屬離子含量。
[Abstract]:The high purity reagent of trichlorotert-butanol semi-hydrate was prepared by sublimation purification method. The effects of sublimation temperature and sublimation time on the process were investigated. The purity and metal ion content of trichlorotert-butanol semi-hydrate before and after sublimation were measured by gas chromatograph (GC) and inductively coupled plasma mass spectrometry (ICP-MS). The samples were detected and analyzed according to the index of Sigma reagent in the United States. The results showed that the yield of trichlorotert-butanol semi-hydrate was 98.2% at 100 鈩,

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