13C qNMR结合DFSS方法测定油品芳碳率

doi:10.11938/cjmr20170102

波谱学杂志 ›› 2017, Vol. 34 ›› Issue (1): 8-15.doi: 10.11938/cjmr20170102

¹³C qNMR结合DFSS方法测定油品芳碳率

马琳鸽, 龙银花

北京低碳清洁能源研究所分析测试中心, 北京 102209

收稿日期:2015-12-25 修回日期:2017-01-04 出版日期:2017-03-05 在线发表日期:2017-03-05
通讯作者: 马琳鸽,Tel:010-57595628,E-mail:malinge@nicenergy.com E-mail:malinge@nicenergy.com
基金资助:
中澳能源联合研究（关键技术联合研究）资助项目（2013DFG61490）

Determination of Aromatic Carbon Mole Ratio in Oil Samples by Quantitative ¹³C NMR Spectroscopy with DFSS Methodology

MA Lin-ge, LONG Yin-hua

Analytical Center, National Institute of Clean-and-Low-Carbon Energy, Beijing 102209, China

Received:2015-12-25 Revised:2017-01-04 Published:2017-03-05 Online:2017-03-05

摘要/Abstract

摘要： 利用六西格玛设计（design for six Sigma，DFSS）方法，通过定量核磁共振碳谱（quantitative carbon nuclearmagnetic resonance spectroscopy，¹³C qNMR）对由11种已知烃类化合物组成的模型油品进行了芳香碳摩尔百分比C（ar）%，简称芳碳率]测定的系统研究，建立了C（ar）%与样品浓度Conc.、弛豫试剂浓度[Cr（acac）₃]和循环延迟D13个参数之间的数学模型，据此模型得到了优化的参数设置：Conc.为180 mg/mL，[Cr（acac）₃]为12 mg/mL，D1为10.5 s.按此设置进行了8组验证实验，其结果重现性较好，相对标准偏差（relative standard deviation，RSD）为0.61%；准确性较高，达到99.0%~100.6%.该方法也可用于其它分析测试方法的系统研究，且实验结果对现行油品芳碳率测定标准中相关参数，如[Cr（acac）₃]和D1的设置能够提出补充性建议.

关键词: 定量核磁共振碳谱(¹³C qNMR), 六西格玛设计(DFSS), 芳碳率, 模型油品

Abstract: Aromatic carbon mole ratios[C(ar)%] in model oil samples, which consisted of 11 saturated/unsaturated compounds with known contents, were determined by quantitative carbon nuclear magnetic resonance spectroscopy (¹³C qNMR) with the design for six Sigma (DFSS) methodology. An empirical model was established between C(ar)% and sample parameters, including sample concentration (Conc.), concentration of relaxation reagent Cr(acac)₃ and relaxation delay (D1). Based on the model, the optimal condition was determined to be at sample concentration 180 mg/mL, concentration of Cr(acac)₃ 12 mg/mL and D1 10.5 s. Eight verification experiments were performed under the optimal condition, and the results showed fairly good repeatability (RSD=0.61%) and accuracy (99.0%~100.6%). The work also gave some supplementary suggestions on parameter settings for the current GB method/ASTM method.

Key words: quantitative carbon nuclear magnetic resonance spectroscopy (¹³C qNMR), design for six Sigma (DFSS), aromatic carbon mole ratios, model oil samples

中图分类号:

O482.53

马琳鸽, 龙银花. ¹³C qNMR结合DFSS方法测定油品芳碳率[J]. 波谱学杂志, 2017, 34(1): 8-15.

MA Lin-ge, LONG Yin-hua. Determination of Aromatic Carbon Mole Ratio in Oil Samples by Quantitative ¹³C NMR Spectroscopy with DFSS Methodology[J]. Chinese Journal of Magnetic Resonance, 2017, 34(1): 8-15.

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¹³C qNMR结合DFSS方法测定油品芳碳率

Determination of Aromatic Carbon Mole Ratio in Oil Samples by Quantitative ¹³C NMR Spectroscopy with DFSS Methodology

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