差示扫描量热法测试PET聚酯Tg、Tc、Tm结果的不确定度评定研究OA
Uncertainty evaluation in the determination of glass transition,crystallization,and melting temperatures of polyethylene terephthalate by differential scanning calorimetry
依据GB/T 19466.1-2004、GB/T 19466.2-2004、GB/T 19466.3-2004使用差示扫描量热仪(DSC)测试聚对苯二甲酸乙二醇酯(PET)聚酯的玻璃化转变温度(Tg)、结晶温度(Tc)、熔融温度(Tm).结合实验室实际情况和测试全过程,分析了对测试结果可能有影响的因素并建立数学模型,对各项不确定度分量进行准确评估研究并确证.通过综合考察测量过程中的各种随机因素(重复性)、天平称量误差、差示扫描量热(DSC)仪器误差、标准物质铟理论值误差、测量结果数据修约等产生的相对不确定度分量,计算出PET聚酯Tg、Tc、Tm测定结果的合成不确定度,综合A、B两个PET聚酯样品的结果,其Tg、Tc、Tm平均不确定度值分别约为±1.0℃、±3.2℃、±2.0℃.通过本不确定度评定研究,明确了关键控制点,进一步指导提升DSC测试的准确度和质量管控方向,也为其他高分子材料的Tg、Tc、Tm准确测试提供了重要参考.
In accordance with the Chinese national standards GB/T 19466.1-2004,GB/T 19466.2-2004,and GB/T 19466.3-2004,differential scanning calorimetry(DSC)was employed to determine the glass transition temperature(Tg),crystallization temperature(Tc),and melting temperature(Tm)of polyethylene terephthalate(PET)-type polyes-ter.To ensure measurement reliability,a comprehensive uncertainty evaluation was conducted based on actual laborato-ry conditions and the full DSC testing procedure.A mathematical model was established to identify,quantify,and com-bine all significant sources of uncertainty.These include repeatability(random variation),balance weighing errors,DSC instrument calibration drift,deviations in the certified reference value of indium(used for temperature calibration),and rounding of reported results.The combined standard uncertainty for each thermal transition was calculated using the law of propagation of uncertainty.Based on measurements of two representative PET samples(A and B),the average ex-panded uncertainties were determined to be approximately±1.0℃for Tg,±3.2℃for Tc,and±2.0℃for Tm.This study not only enhances the metrological traceability and reliability of DSC measurements for PET but also identifies criti-cal control points,such as calibration accuracy and sample preparation,that significantly influence result quality.The methodology and findings provide a robust framework for uncertainty assessment in the thermal analysis of other semi-crystalline polymers.
叶淋泉;曾乐;兰孟琦
华润化学材料科技股份有限公司,江苏 常州 213033华润化学材料科技股份有限公司,江苏 常州 213033华润化学材料科技股份有限公司,江苏 常州 213033
化学化工
聚对苯二甲酸乙二醇酯差示扫描量热仪玻璃化转变温度结晶温度熔融温度不确定度评定
polyethylene terephthalatedifferential scanning calorimetryglass transition temperaturecrystallization temperaturemelting temperatureevaluation of uncertainty
《中国塑料》 2026 (4)
90-95,6
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