摘要
依据标准GB/6730.62—2005《铁矿石钙、硅、镁、钛、磷、锰、铝和钡含量的测定波长色散X射线荧光光谱法》测定铁矿石中SiO_(2)含量。将SiO_(2)质量分数为8.78%的含砷铁矿标准样品YSBC 14721—98作为质控样品,不同人员不同时间对铁矿质控样品进行测量得到20个数据,离群值检验后,依据国标GB/T 27407—2010和GB/T 27411—2012中评定过程进行Top-Down技术控制图法不确定度评定。期间精密度在重复性和再现性标准偏差之间,评价合理;平均偏倚和“0”没有显著性差异,无需校正。检测某铁矿样品,SiO_(2)质量分数5.24%,由期间精密度带来的不确定度为0.0256%,由偏倚带来的不确定度为0.0313%。由这两项合成的标准不确定度u为0.0404%,取包含概率p=95%,包含因子k=2,扩展不确定度U为0.08%。评定方法既得到了不确定度,又和日常质控结合起来,保证了检测质量,值得实验室推广使用。
According to the standard method GB/6730.62-2005,iron ores-determination of calcium,silicon,magnesium,titanium,phosphorus,manganese,aluminum and barium content-wavelength dispersive X-ray fluorescence spectrometry method,the content of SiO_(2) in iron ores was determined.The certified reference material YSBC 14721-98,which contains 8.78%SiO_(2),was taken as the quality control sample,and 20 datas were obtained by measuring the quality control sample at different time by different operator,after outlier testing,according to the GB/T 27407-2010 and the GB/T 27411-2012,the uncertainty was evaluated by Top-Down technical control chart method.The intermediate precision was between the standard deviation of repeatability and reproducibility,which was reasonable.An iron ore sample was determined,the content of SiO_(2) was 5.24%,the uncertainty was 0.0256%,the uncertainty u(b)was 0.0313%,the standard uncertainty u was 0.0404%,under the coverage probability p=95%and the coverage factor k=2,the expanded uncertainty U was 0.08%.This evaluation method not only obtains the uncertainty,but also combines with the daily quality control to ensure the detection quality,which should promote using in the laboratories.
作者
冯丽丽
丁仕兵
徐小茗
管嵩
吴雅俊
宋飞
Feng Lili;Ding Shibing;Xu Xiaoming;Guan Song;Wu Yajun;Song Fei(Technology Center of Qingdao Customs,Qingdao 266500,China)
出处
《云南化工》
CAS
2024年第6期96-99,共4页
Yunnan Chemical Technology
