|
|
|
| Evaluation of Uncertainty in Measurement of Purity of Phthalic Anhydride by Gas Chromatography |
| DING Xin-yan1,2,ZHOU Ji3,WANG Wei1,2,YAN Hai-jun3,BAI Miao-miao1,2 |
1. School of Chemistry and Chemical Engineering, Yulin University, Yulin, Shaanxi 719000, China
2. Shaanxi Key Laboratory of Low Metamorphic Coal Clean Utilization,Yulin, Shaanxi 719000, China
3. National Coal and Salt Chemical Product Quality Supervision and Inspection Center, Yulin, Shaanxi 719000, China |
|
|
|
|
Abstract According to GB/T 15336-2013 “phthalic anhydride”, the purity of phthalic anhydride was determined by gas chromatography, and the mathematical model was established. The sources of uncertainty in the determination process were analyzed and evaluated. The synthetic uncertainty of purity measurement results of phthalic anhydride was obtained by calculating the uncertainty caused by repeatability, sample mass, solvent volume and response factor. The experimental results showed that the main factors affecting the uncertainty was solvent volume, followed by response factor and sample quality. Through the evaluation of uncertainty, it was helpful to improve the reliability of the test results and can provide theoretical basis for the accurate determination of phthalic anhydride purity.
|
|
Received: 12 November 2020
Published: 19 September 2022
|
|
|
|
|
|
［1］GB/T 15336-2013 邻苯二甲酸酐［S］.
［2］CNAS-CL01-G003 2019 测量不确定度的要求［S］.
［3］孙晓辉, 程绍尊, 张玉玲. 邻苯二甲酸酐纯度分析方法的改进［J］. 齐鲁石油化工, 2003, 31(2): 178-180.
Sun X H, Cheng S Z, Zhang Y L. Improvement of purity analysis method for phthalic anhydride ［J］. Qilu Petrochemical, 2003, 31 (2): 178-180.
［4］曹文婷, 宋寅生, 曹杰. 毛细管气相色谱法测定工作场所空气中邻苯二甲酸酐［J］. 江苏预防医学, 2012, 23(3): 64-65.
Cao W T, Song Y S, Cao J. Determination of phthalic anhydride in workplace air by capillary gas chromatography［J］. Jiangsu Preventive Medicine, 2012, 23 (3): 64-65.
［5］GB/T 27418-2017 测量不确定度评定与表示［S］.
［6］JJF 1135-2005 化学分析测量不确定度评定［S］.
［7］陈凌峰. 抽样引起的测量不确定度评定［J］. 计量学报, 2020, 41(7): 891-896.
Chen L F. Evaluation of measurement uncertainty caused by sampling ［J］. Acta Metrologica Sinica, 2020, 41 (7): 891-896.
［8］丁红红, 王韦斌, 解卫. 冷原子吸收测汞仪检出限检定结果的不确定度评定［J］. 计量与测试技术, 2020, 47(7): 100-101.
Ding H H, Wang W B, Xie W. Evaluation of uncertainty of detection limit of mercury detector by cold atomic absorption spectrometry ［J］. Metrology and Testing Technology, 2020, 47 (7): 100-101.
［9］贾未鸣, 高旭锋, 凌凤香, 等. 微晶蜡含油量不确定度评估［J］. 计量学报, 2020, 41(7): 886-890.
Jia W M, Gao X F, Ling F X, et al. Uncertainty Evaluation of oil content in microcrystalline wax ［J］. Acta Metrologica Sinica, 2020, 41 (7): 886-890.
［10］马浩淼, 吴海, 王德发, 等. 面积归一法测定萜烯试剂纯度［J］. 计量学报, 2018, 39(5): 736-740.
Mao H M, Wu H, Wang D F, et al. Determination of terpene reagent purity by area normalization method ［J］. Acta Metrologica Sinica, 2018, 39 (5): 736-740.
［11］吕雅竹, 赵瑞, 李德红, 等. X射线剂量当量仪校准因子不确定度评估［J］. 计量学报, 2020, 41(9): 1133-1137.
Lv Y Z, Zhao R, Li D H, et al. Evaluation of uncertainty in calibration factor of X-ray dose equivalent instrument ［J］. Acta Metrologica Sinica, 2020, 41 (9): 1133-1137.
［12］王文佳, 李东刚, 吴凡, 等. 车用乙醇汽油中乙醇含量测量不确定度的评定［J］. 化学工程师, 2010, 2(59): 59-62.
Wang W J, Li D G, Wu F, et al. Evaluation of uncertainty in measurement of ethanol content in ethanol gasoline［J］. Chemical Engineer, 2010, 2 (59): 59-62.
［13］JJG-196-2006 《常用玻璃量器检定规程》［S］.
［14］高吉. 气相色谱法测定车用汽油中苯含量的不确定度评定［J］. 计量与测试技术, 2012, 39(6): 45-49.
Gao J. Risk Evaluation of uncertainty in determination of benzene in gasoline by gas chromatography ［J］. Metrology and Testing Technology, 2012, 39 (6): 45-49.
［15］刘卫. 汽油有机组分含量计量技术研究［D］. 北京: 中国石油大学(北京), 2008.
［16］王宏涛, 王汉斌, 陈晓怀, 等, 测量不确定度引起的批量产品检验误判风险评估［J］. 计量学报, 2017, 38(5): 559-562.
Wang H T, Wang H B, Chen X H, et al. Risk assessment of batch product inspection misjudgment caused by measurement uncertainty ［J］. Acta Metrologica Sinica, 2017, 38 (5): 559-562.
［17］黄亮, 张伟, 黄挺, 等. 肌酐纯度标准物质的定值方法及其不确定度评定研究［J］. 分析测试学报, 2014, 33(7): 840-846.
Huang L, Zhang W, Huang T, et al. Research on a Certified Reference Material for Purity of Creatinine and Its Uncertainty Evaluation［J］. Journal of Instrumental Analysis, 2014, 33(7): 840-846.
［18］闫文灿, 王池, 裴全斌, 等. 气相色谱法测量天然气热值的不确定度评定［J］. 计量学报, 2018, 39(2): 280-284.
Yan W C, Wang C, Pei Q B, et al. Uncertainty Evaluation on the Calorific Value of Natural Gas by GC［J］. Acta Metrologica Sinica, 2018, 39(2): 280-284.
［19］王家兴, 张会成, 高波, 等. 基于CFR辛烷值测量系统的不确定度评定［J］. 计量学报, 2018, 39(4): 583-587.
Wang J X, Zhang H C, Gao B, et al. Uncertainty Evaluation for CFR Octane Number Testing System of Gasoline［J］. Acta Metrologica Sinica, 2018, 39(4): 583-587.
［20］倪晓丽. 化学分析中不确定度的评估指南［M］. 北京: 中国计量出版社, 2008.
［21］谷瑞丽, 刘智勇, 姚晓洁, 等. 气相色谱法测定熏煮肠火腿制品脱氢乙酸含量不确定度评定［J］. 河南预防医学杂志, 2020, 31(10): 735-738.
Gu R L, Liu Z Y, Yao X J, et al. Evaluationof uncertainty in the determination of dehydroacetic acid in smoked and cooked sausage ham products by gas chromatography［J］. Henan Journal of Preventive Medicine, 2020, 31(10):735-738. |
|
|
|
2022, Vol. 43 
