间二甲苯磺化的产物有3,5-间二甲苯磺酸和2,4-间二甲苯磺酸两种异构体。它们不能挥发,可使之转化成有一定挥发性的间二甲苯磺酰氟,然后用气相色谱分离,定性、定量。 1.化学处理:称样品1克和内标对甲苯磺酸0.3克于50毫升的烧杯中,加入2毫升二甲基甲酰胺作溶剂,再缓缓加入1毫升氯化亚砜,将反应物一并倒入三角烧瓶加热至沸,保温20分,冷却后以细流倒在冰块上,用倾析法洗涤,得结晶磺酰氯,再加二甲基甲酰胺3毫升,氟化钾 Meta-xylene sulfonated products are 3,5-m-xylene sulfonic acid and 2,4-m-xylene sulfonic acid two isomers. They can not be volatile, can be converted into a certain volatile m-xylene sulfonyl fluoride, and then separated by gas chromatography, qualitative and quantitative. 1. Chemical treatment: Weigh the sample 1 g and the internal standard p-toluenesulfonic acid 0.3 g in 50 ml beaker, add 2 ml dimethylformamide as a solvent, and then slowly add 1 ml of thionyl chloride, the reactant Poured into the conical flask were heated to boiling, incubated for 20 minutes, cooled down to a thin stream on ice, washed with a decantation to give crystalline sulfonyl chloride, plus dimethylformamide 3 ml, potassium fluoride