为合成新型精细化工品和功能高分子中间体,研究了磷钨杂多酸(PW)催化下芘与乙酰氯的Friedel-Craft酰基化反应,合成了新型精细化工产品及功能高分子中间体1-乙酰芘。用GC法考察了不同反应条件对1-乙酰芘收率和选择性的影响,当溶剂为1,2-二氯乙烷,催化剂PW质量分数为8%,n(芘)∶n(乙酰氯)=1∶6,反应温度60℃,反应时间8h时,1-乙酰芘收率可达79.2%,选择性100%。且PW对环境污染小,并可循环使用。采用萃取、重结晶等方法得到了1-乙酰芘纯品,通过GC、GC/MS、FT IR和1 H NMR对该产物进行了定性和定量分析。
Three new reduced Schiff base derived from o-vanillin and amino acids such as alanine, leucine, and phenylalanine are prepared through condensation, reduction, and acidification. Their Ni(Ⅱ) complexes are also synthesized by the reduction of Schiff base, respectively.All new synthesized compounds are characterized by element analysis, atomic absorption spectrophotometry, and infrared spectra. Meanwhile the thermal stability and DRS UV/Vis of three complexes are also studied.
用亚甲基蓝电荷转移光度法测定红霉素,以二次石英蒸馏水为溶剂,红霉素与亚甲基蓝在常温下进行电荷转移反应生成1∶1稳定的配合物,用可见及紫外分光光度计于最大波长678 nm测定其吸光度。实验表明:此法灵敏度高(ε=1.59×104L/(mol.cm)),精密度较好(对25 mL 5.0×10-3mg/mL红霉素9次,RSD=3.0%)。红霉素的浓度在0.0008～0.0250 mg/mL范围内服从Beer定律,方法的检出限为0.11μg/mL。该方法可靠,重现性好,可用于红霉素肠溶片和兽用红霉素含量的测定。
