红外光谱法测定柴油中脂肪酸甲酯的检出限及不确定度评定

doi:10.3969/j.issn.1000-1158.2021.08.21

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摘要柴油中脂肪酸甲酯含量的测定广泛采用红外光谱法,针对此方法的检测能力和准确性进行了研究。试验测定红外光谱法检测柴油中脂肪酸甲酯的检出限和定量限分别为0.0066g/L和0.0220g/L,加标回收率为99.2%~101.3%,结果表明试验方法具备良好的准确性,能够准确灵敏地检测柴油中脂肪酸甲酯。测定的合成相对标准不确定度为0.0123(置信概率取95%,包含因子k=2),脂肪酸甲酯含量为(3.960±0.097)g/L。分析结果表明标准溶液配制和待测样品配制为引入不确定度的主要因素。

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	郭士刚
	凌凤香
	高旭锋

关键词 ：计量学, 脂肪酸甲酯, 生物柴油, 红外光谱, 检出限, 不确定度

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.

Key words： metrology fatty acid methyl ester biodiesel infrared spectrum detection limit uncertainty

收稿日期: 2019-09-02 发布日期: 2021-08-20

PACS:

TB99

基金资助:中国石油化工集团有限公司资助项目(117012)

通讯作者: 凌凤香(1966-),女,山西太谷人,中国石油化工股份有限公司大连石油化工研究院教授级高级工程师,从事石油炼制催化材料、油品分析表征、标准化及基础研究。Email:lingfengxiang.fshy@sinopec.com E-mail: lingfengxiang.fshy@sinopec.com

作者简介: 郭士刚(1991-),男,内蒙古赤峰人,中国石油化工股份有限公司大连石油化工研究院助理研究员,研究方向为石油产品分析表征、检测技术和特种油品开发及标准化。Email:guoshigang.fshy@sinopec.com

引用本文:

郭士刚,凌凤香,高旭锋. 红外光谱法测定柴油中脂肪酸甲酯的检出限及不确定度评定[J]. 计量学报, 2021, 42(8): 1115-1120.
GUO Shi-gang,LING Feng-xiang,GAO Xu-feng. Evaluation of Detection Limit and Uncertainty of Determination of Fatty Acid Methyl Esters in Diesel Fuels by Infrared Spectrometric Method. Acta Metrologica Sinica, 2021, 42(8): 1115-1120.

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