石油炼制与化工 ›› 2024, Vol. 55 ›› Issue (5): 165-171.

• 分析与评定 • 上一篇    

差示扫描量热法测定石蜡熔点的研究

李淑杰,王刚,李奕睿,张立军,马丽   

  1. 中国石油石油化工研究院大庆化工研究中心
  • 收稿日期:2023-08-17 修回日期:2024-02-05 出版日期:2024-05-12 发布日期:2024-05-06
  • 通讯作者: 李淑杰 E-mail:lsjwy459@163.com

RESEARCH ON DIFFERENTIAL SCANNING CALORIMETRY METHOD FOR THE DETERMINATION OF MELTING POINT OF PARAFFIN WAX


  • Received:2023-08-17 Revised:2024-02-05 Online:2024-05-12 Published:2024-05-06

摘要: 采用差示扫描量热(DSC)技术,模拟石蜡熔点(冷却曲线法)测试过程,测定石蜡的熔点。研究了起始温度、终止温度、吹扫气(氮气)流量、升降温速率、试样质量、恒温时间、样品制备方式、升降温次数等对测试结果的影响,确定了DSC法测定石蜡熔点的适宜条件,考察了DSC法与标准方法(GB/T2539—2008)的偏倚。结果表明,采用DSC法测定石蜡熔点时的升温速率宜为10℃/min,降温速率宜为5℃/min,试样在高于预估熔点20~30℃下熔融时间不应超过1h。通过采用6台不同型号的DSC仪器对14个牌号石蜡样品进行测试,计算出DSC法与标准方法的偏倚为-1.14℃。DSC法操作简单、试样用量少、检测速率快、重复性好,可作为控制分析手段,快速准确地测定石蜡的熔点。

关键词: 差示扫描量热法, 熔点, 石蜡, 偏倚

Abstract: The melting point of paraffin wax was determined by means of differential scanning calorimetry (DSC) method, simulating the measuring process of melting point of paraffin wax(cooling curve method). The effects of starting and stopping temperatures, nitrogen purge gas flow rate, temperature rising and falling rate, sample mass, constant temperature time, sample preparation method, and temperature rising and falling times on the measurement results were studied,the suitable conditions for determining the melting point of paraffin wax by DSC method were determined, and the bias between DSC method and standard method (GB/T 2539-2008) was investigated. The results showed that the heating rate and cooling rate was 10 ℃/min and 5 ℃/min respectively when the melting point of paraffin wax was determined by DSC method, and the melting time should not exceed 1 h when the melting point was 20-30 ℃ above the predicted melting point. By testing 14 kinds of paraffin wax samples with 6 kinds of DSC instruments, the deviation between DSC and standard method was calculated to be -1.14 ℃. DSC method is a simple, rapid and repeatable method for determining the melting point of paraffin wax,and can be used as a control analysis method to quickly and accurately determine the melting point of paraffin wax.

Key words: differential scanning calorimetry method, melting point, paraffin wax, deviation