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为进一步确定YC/T 207—2014标准测量方法的重复性限(r)和再现性限(R),利用2016年国家烟草质量监督检验中心实施的YC/T 207—2014标准测量方法共同实验,对50家实验室的3个水平样品检测结果进行柯克伦和格拉布斯离群值检查,按照GB/T 6379.2—2004/ISO 5725-2:1994的方法获得了烟用纸张中甲醇、丁酮、苯、1-乙氧基-2-丙醇、乙酸正丁酯和邻二甲苯6种溶剂残留测定结果的重复性和再现性精密度评价结果。结果表明:在重复性条件下,6个溶剂残留指标测定结果的相对重复性标准差(RSDr)在1.7%~4.5%之间,满足YC/T 207—2014所规定重复性条件下10%的允许差要求;在再现性条件下,除了最低质量分数水平的1-乙氧基-2-丙醇和邻二甲苯两项指标外,溶剂残留其他指标的相对再现性标准差(RSDR)在5.6%~14.4%之间。由于YC/T 207—2014标准方法精密度与测量水平具有良好的线性关系,最终以重复性标准差(Sr)、再现性标准差(SR)对应测量水平均值的线性函数关系作为精密度的评价结果。
To further determine the repeatability limit (r) and reproducibility limit (R) of the YC / T 207-2014 standard measurement method, the YC / T 207-2014 standard measurement method conducted by the National Tobacco Quality Supervision and Testing Center of 2016 was used to experiment together. Kirkland and Grubbs outliers were tested on the results of three horizontal samples in 50 laboratories. Methanol, methyl ethyl ketone, ethyl acetate, Benzene, 1-ethoxy-2-propanol, n-butyl acetate and o-xylene 6 kinds of solvents Residue determination of reproducibility and reproducibility of the results of the evaluation of precision. The results showed that the relative standard deviation of repeatability (RSDr) of the six solvent residue indexes were between 1.7% and 4.5% under the repeatability conditions, and the repeatability of YC / T 207-2014 under the conditions of 10% Allow poor requirements; Under reproducibility conditions, the relative standard deviation of reproducibility (RSDR) of other indicators of solvent residue except for two indicators of 1-ethoxy-2-propanol and o-xylene at the lowest quality score is between 5.6% ~ 14.4% between. Since the YC / T 207-2014 standard method has a good linear relationship between the precision and the measurement level, the linear function of the standard deviation (SR) and reproducibility standard deviation result.