水分对DSC法熔点分析的影响研究

刘毅; 吴锐; 覃玲; 徐鹏; 郭贤辉; 林兰

doi:10.13748/j.cnki.issn1007-7693.20231443

水分对DSC法熔点分析的影响研究

Study on the Influence of Moisture on DSC Melting Point Analysis

摘要

摘要:
目的研究差示扫描量热法(differential scanning calorimetry，DSC)熔点分析中吸附水分的影响。
方法常规DSC法熔点分析起始温度为室温30 ℃，升温速率为10 ℃·min⁻¹，气氛为氮气，干燥气为50 mL·min⁻¹；优化后DSC法熔点分析起始温度为熔融温度前20 ℃，升温速率为1 ℃·min⁻¹，其余参数不变。
结果无须干燥处理试样，常规DSC法熔点分析可以准确检测水分含量分别为4.3%、5.3%和6.1%的咪唑、盐酸去氧肾上腺素和甲硫酸新斯的明试样，方法优化后进一步弱化水分影响，可以准确分析相应水分含量分别为9.0%、6.0%和7.1%的试样。
结论 DSC法熔点分析无须干燥处理样品，常规检测一般试样与需要提前干燥样品的毛细管法无差别，优化后的方法进一步降低吸附水分的影响，方法适用性更广。

Abstract:
OBJECTIVE To study on the influence of moisture on differential scanning calorimetry(DSC) melting point analysis.
METHODS In the general method of DSC melting point analysis, the melting range with 30 ℃ of start temperature and 10 ℃·min⁻¹ heating rate, the atmosphere was nitrogen and the dry gas flow was 50 mL·min⁻¹. In the optimization method, the start temperature was 20 ℃ before melting temperature, the heating rate was adjusted to 1 ℃·min⁻¹, and the other parameters remained unchanged.
RESULTS Without drying test samples, the melting point could be detected accurately in the general method of DSC melting point analysis for the imidazole, norepinephrine hydrochloride and methylthioneostigmine samples with moisture content of 4.3%, 5.3% and 6.1% respectively, and in the optimization method of weakening the influence of moisture, the melting point could be analyzed exactly for the homologous samples with moisture content of 9.0%, 6.0% and 7.1% respectively.
CONCLUSION The DSC method for melting point analysis need not to dry samples, and there is no difference between the conventional DSC method and the capillary method that need to pre dry samples. The optimized DSC method further reduced the impact of adsorbed moisture and has wider applicability.

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