差示扫描量热单峰法测定苯氯乙酮纯度

Determination of the purity of chloroacetophenone by the monpeak method of differential scanning calorimetry

利用差示扫描量热单峰法测定苯氯乙酮的纯度。讨论了在不同样品质量和升温速率下苯氯乙酮纯度测定结果的差异,并与高效液相色谱法测定结果进行比较。分析表明:两种方法测定结果基本一致,偏差为0.01%;测定不同质量的样品,其纯度测定值最大相差0.07%;不同升温速率下,试样的纯度测定值最大相差0.72%;当升温速率控制在1.0~2.0℃/min,取样质量控制在2.0~3.0 mg时,测定结果准确度最高。该法操作简便,测定时间较短。

The purity of chloroacetophenone was measured by the monpeak method of differential scanning calorimetry.The test results with different sample mass and different heating rates were discussed.Meanwhile,the purity of chloroacetophenone was also tested by high performance liquid chromatography.The difference of the determination results was compared between differential scanning calorimetry and high performance liquid chromatography,which showed the same approximately,the result determined by differential scanning calorimetry measurement was smaller 0.01%than that determined by high performance liquid chromatography.The maximum difference value of the purity with different samples dosage was 0.07%,and the maximum difference value at different heating rates was 0.72%.The differential scanning calorimetry perfected best when the heating rate was 0.5-2.0℃/min and the sample dosage was 2.0-3.0 mg.This method is simple,fast and accuracy for the measurement of chloroacetophenone purity.