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| Evaluation of Detection Limit and Uncertainty of Determination of Fatty Acid Methyl Esters in Diesel Fuels by Infrared Spectrometric Method |
| GUO Shi-gang,LING Feng-xiang,GAO Xu-feng |
| Dalian Research Institute of Petroleum and Petrochemicals,SINOPEC,Dalian,Liaoning 116045,China |
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Abstract Infrared spectroscopy is widely used in the determination of fatty acid methyl ester content in diesel oil, and the detection ability and accuracy of this method have been studied. The limits of detection and quantification of fatty acid methyl ester in diesel oil by infrared spectroscopy were 0.0066g/L and 0.0220g/L, respectively, and the recoveries were 99.2%~101.3%. By evaluating detection limit, the method had good accuracy, could accurately and sensitively detect fatty acid methyl ester in diesel. The combined related standard uncertainty of determination of fatty acid methyl esters in diesel fuels by infrared spectrometric method was 0.0123, and the measurement result of fatty acid methyl esters was (3.960±0.097)g/L, under the condition that the fiducial probability was 95% and the coverage factor k was 2. The results showed that the sources of uncertainty were mainly derived from standard weighing and sample volume.
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Received: 02 September 2019
Published: 20 August 2021
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［1］石赛南, 金邻豫, 裴瑞敏, 等. 生物柴油中脂肪酸甲酯的成分分析 ［J］. 化学研究, 2016, 27 (1): 85-87.
Shi S N, Jin L Y, Pei R M, et al. Analysis of fatty acid methyl ester in the biodiesel ［J］. Chemical Research, 2016, 27 (1): 85-87.
［2］林海, 关剑锋, 毛容妹, 等. 全二维气相色谱法测定柴油和生物柴油混合燃料中7种脂肪酸甲酯含量 ［J］. 现代化工, 2016, 36 (2): 188-190.
Lin H, Guan J F, Mao R M, et al. Determination of seven fatty acid methyl esters in diesel-biodiesel blend fuel by comprehensive two-dimensional gas chromatogr-aphy ［J］. Modern Chemical Industry, 2016, 36 (2): 188-190.
［3］GB/T 23801—2009中间馏分油中脂肪酸甲酯含量的测定红外光谱法 ［S］. 北京: 中国标准出版社, 2009.
［4］李率, 蔺建民, 张永光. 《中间馏分油中脂肪酸甲酯含量的测定红外光谱法》 解读 ［J］. 石油商技, 2011, 29 (6): 76-79.
Li S, Lin J M, Zhang Y G. Interpretation of Deter-mination of fatty acid methyl esters (FAME) in middle distillates by infrared spectroscopy method ［J］. Petroleum Products Application Research, 2011, 29 (6): 76-79.
［5］张疆兵. 傅立叶变换红外光谱仪在测定柴油中脂肪酸甲酯中的应用 ［J］. 中国石油和化工标准与质量, 2013, 23 (1): 45-46.
Zhang J B. Application of Fourier transform infrared spectrometer in Determination of fatty acid methyl esters (FAME) in middle distillates ［J］. China Petroleum and Chemical Standard and Quality, 2013, 23 (1): 45-46.
［6］郭登峰, 盛梅, 罗士平. 气相色谱法测定生物柴油中多种脂肪酸甲酯 ［J］.中国油脂, 2004, 29 (4): 44-46.
Guo D F, Sheng M, Luo S P. Determination of fatty acid methyl esters in biodiesel by gas chromatography ［J］. China Oils and Fats, 2004, 29 (4): 44-46.
［7］Armbruster D A, Tillman M D, Hubbs L M. Limit of detection (LOD)/limit of quantitation (LOQ): Compa-rison of the empirical and the statistical methods exempli-fied with GC-MS assays of abused drugs ［J］. Clinical Chemistry, 1994, 40 (71): 1233-1238.
［8］徐金龙, 刘中勇, 华斌, 等. 分析化学中检出限问题探讨 ［J］.检验检疫学刊, 2012, 22 (6): 74-76.
Xu J L, Liu Z Y, Hua B, et al. Discussion of Detection Limit Concept Question in Analytical Chemistry ［J］. Journal of Inspection and Quarantine, 2012, 22 (6): 74-76.
［9］田强兵. 分析化学中检出限和测定下限的探讨 ［J］. 化学分析计量, 2007, 16 (3): 72-73.
Tian Q B. Discussion on detection limit and minimum detection limit in analytical chemistry ［J］. Chemical Analysis and Meterage, 2007, 16 (3): 72-73.
［10］陈勇. 浅谈检测限 ［J］. 中国现代药物应用, 2013, 7 (16): 256-257.
Chen Y. Brief talk about detection limit ［J］. Chinese Journal of Modern Drug Application. 2013, 7 (16): 256-257.
［11］丰达明. 分析化学中的检出限和测定下限 ［J］. 化学通报, 1982, 5 (11): 42-52.
Feng D M. Limits of detection and minimum detection limit in analytical chemistry ［J］. Chemistry, 1982, 5 (11): 42- 52.
［12］王艳洁, 那广水, 王震. 检出限的涵义和计算方法 ［J］. 化学分析计量, 2012, 21 (5): 85-88.
Wang Y J, Na G S, Wang Z. Connotation and Calculation Methods of Detection Limit ［J］. Chemical Analysis and Meterage, 2012, 21 (5): 85-88.
［13］邱英, 彭延岭. 测量不确定度评定与表示 ［J］. 机械工程师, 2007, (4): 60-62.
Qiu Y, Peng Y L. Evaluation and expression of meas-urement uncertainty ［J］. Mechanical Engineer, 2007, (4): 60-62.
［14］邓自西. 气相色谱法和高效液相色谱法分析中不确定度的评定 ［J］. 色谱, 2004, 22 (5): 568-568.
Deng Z X. Evaluation of uncertainty in gas chromato-graphy and high performance liquid chromatography ［J］. Chinese Journal of Chromatography, 2004, 22 (5): 568-568.
［15］Barwick V J, Ellison S I, Rafferty M J, et al. The evaluation of measurement uncertainty from method validation studies. Part 2: The practical application of a laboratory protocol ［J］. Accreditation and Quality Assur-ance, 2000, 5 (3): 104-113.
［16］Michèle Désenfant, Priel M. Road map for measurement uncertainty valuation ［J］. Measurement, 2006, 39 (9): 841-848.
［17］王伟, 潘春秀. 光度法测定钢铁及合金中锰含量的不确定度评定 ［J］. 计量学报, 2005, 26 (2): 189-192.
Wang W, Pan C X. Uncertainty Evaluation of Spectro-photometric Determination of Manganese in Steel and Alloy ［J］. Acta Metrologica Sinica, 2005, 26 (2): 189-192.
［18］Rui-Hua K E. Evaluation of uncertainty in the measure-ment for chemical content ［J］. Metallurgical Analysis, 2004, 24 (1): 63-63.
［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］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): 138-142.
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): 138-142.
［21］陈爽, 徐接胜. 关于检出限的定义、 分类及估算方法的探讨 ［J］. 广州化工, 2014, 42 (18): 137-139.
Chen S, Xü J S. Discussion on the Definition,Classification and Estimation of Detection Limit ［J］. Guangzhou Chemical Industry, 2014, 42 (18): 137-139.
［22］高若梅, 刘鸿皋. 检出限概念问题讨论—IUPAC及其它检出限定义的综合探讨和实验论证 ［J］. 分析化学, 1993, 21 (10): 1232-1236.
Gao R M, Liu H G. Discussion on the Concept of Detection Limit—A Comprehensive Discussion and Experimental Demonstration on the Definition of IUPAC and Other Definition of Detection Limits ［J］. Chinese Journal of Analytical Chemistry, 1993, 21 (10): 1232-1236.
［23］丘晖饶, 庞晋山. 电位滴定法测定润滑油酸值不确定度评估 ［J］. 计量学报, 2019, 40 (5): 937-940.
Qiu H R, Pang J S. Uncertainty Evaluation for the Determination of the Acid Number of Lubricant Oils by Potentiometric Titration ［J］. Acta Metrologica Sinica, 2019, 40 (5): 937-940.
［24］陈凌峰. 标准不确定度A类评定中极差法的深入讨论 ［J］. 计量学报, 2019, 40 (2): 173-178.
Chen L F. The Further Discussion of the Range Method in the Type A Evaluation of Sstandard Uncertainty ［J］. Acta Metrologica Sinica, 2019, 40 (2): 173-178. |
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2021, Vol. 42 
