CN112229939B - 液相色谱法分析检测原油中十八烷基二甲基甜菜碱的方法 - Google Patents
液相色谱法分析检测原油中十八烷基二甲基甜菜碱的方法 Download PDFInfo
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Abstract
本发明公开了一种液相色谱法分析检测原油中十八烷基二甲基甜菜碱的方法,包括(1)样品前处理:将待检测原油样品与正己烷以1:1的体积比混匀后再采用等体积的无乙醇/水混合液萃取上述原油/正己烷混合液中的甜菜碱表面活性剂,静置分层,萃取液作为进样样品;(2)色谱条件:色谱柱为25 cm C18色谱柱;流动相为乙腈/水的混合液(体积比3/2);采用质谱检测器,ESI源,正模式检测;(3)外标法定量:测定萃取液中十八烷基二甲基甜菜碱的峰面积,依据线性关系计算原油样品中十八烷基二甲基甜菜碱的浓度。该方法具有准确可靠,重复性好,灵敏性高等特点,为驱油剂在油藏环境中的运移规律的研究提供技术支撑。
Description
技术领域
本发明涉及一种原油中十八烷基二甲基甜菜碱两性表面活性剂的测定方法,尤其涉及一种采用高效液相色谱法测定原油中十八烷基二甲基甜菜碱的方法,属于分析化学技术领域。
背景技术
表面活性剂在三次采油中发挥着重要作用,其作用机理在于有效降低油水界面张力,增强体系乳化性能,进而提高原油采收率。十八烷基二甲基甜菜碱两性表面活性剂近年来以其优异的界面性能被广泛的应用于三次采油领域。十八烷基二甲基甜菜碱两性表面活性剂的结构是由十八烷基二甲基季铵盐阳离子基团与羧酸根阴离子基团两部分组成的两性表面活性剂,其结构式如下:
因为十八烷基二甲基甜菜碱两性表面活性剂疏水性较强,在水相分配较少,易于进入油相,因此,十分有必要建立原油中十八烷基二甲基甜菜碱两性表面活性剂的分析检测方法,为驱油剂在油藏环境中的运移规律的研究提供技术支撑。然而,截止目前,鲜有针对原油中甜菜碱两性表面活性剂的分析检测方法。
发明内容
本发明的目的是提供一种液相色谱分析检测原油中十八烷基二甲基甜菜碱两性表面活性剂的方法。
本发明液相色谱分析检测原油中十八烷基二甲基甜菜碱的方法,包括以下内容:
(1)待测原油样品前处理
将待检测原油样品与正己烷以1:1的体积比混匀,得到原油/正己烷混合液;再采用乙醇/水混合液(体积比1/1)萃取上述原油/正己烷混合液中的甜菜碱表面活性剂,静置分层,萃取液作为进样样品;乙醇/水混合液与原油/正己烷混合液的体积比为1:1。
(2)色谱条件
色谱柱:25 cm C18色谱柱;
流动相:乙腈/水的混合液(体积比3/2),流速1.0 mL/min;
检测器:质谱检测器,ESI源,正模式检测;
(3)标准线性回归曲线
以原油为基质溶剂,分别配制10、20、50、100、200、500、1000 mg/L等系列不同浓度的十八烷基二甲基甜菜碱原油溶液,作为标准曲线待测原油样品,并进行步骤(1)样品前处理。
在上述色谱条件下进样水乙醇/水萃取液,进样量20 μL,测定十八烷基二甲基甜菜碱的色谱峰面积,以峰面积积分值为纵坐标,以原油中十八烷基二甲基甜菜碱浓度为横坐标,经线性回归处理得标准曲线(见图1)。
结果表明,在50~500 mg/L范围内,原油中十八烷基二甲基甜菜碱的浓度与色谱峰面积之间具有良好的线性关系,具体线性方程为:
Y = 98992000 + 9638310 X,线性相关系数R = 0.99968
其中,X——十八烷基二甲基甜菜碱的浓度,单位mg/L
Y——质谱色谱峰面积,单位:Intens。
(4)外标法定量
将经步骤(1)前处理的待测原油样品在上述色谱条件下进样,进样量20 μL,测定萃取液中十八烷基二甲基甜菜碱的峰面积,依据线性关系计算原油样品中十八烷基二甲基甜菜碱的浓度。
(5)检出限测定
在上述色谱条件下,将原油中十八烷基二甲基甜菜碱浓度不断稀释,测定其质谱色谱峰响应强度,确定了该方法检出限可以低至20 mg/L,证实了该方法的灵敏性。
(6)重复性测试
在上述色谱条件下,将原油中十八烷基二甲基甜菜碱浓度为100 mg/L的样品分别在第一天、第三天、第五天进样,测定质谱色谱峰面积,计算检测浓度,考察数据的重复性。经测定,检测浓度分别为90.26、87.49、92.34 mg/L。经计算,相对标准偏差为2.70%,较小,说明数据的重复性很好。
(7)油井采出液加标回收率实验
往6AT235、6AT216、6A237三组原油中添加100 ppm十八烷基二甲基甜菜碱,测定峰面积,扣除本底,依据线性关系,计算测定浓度。测定浓度对比加标浓度100 ppm,获得不同原油中十八烷基二甲基甜菜碱的加标回收率,见表1:
由表1可以看出,三组原油样品中十八烷基二甲基甜菜碱的加标回收率均在84.62%~91.39%之间,证实了所提供的原油中十八烷基二甲基甜菜碱的液相色谱分析检测方法的可靠性。
综上所述,本发明采用高效液相色谱法测定原油中十八烷基二甲基甜菜碱,具有准确可靠,重复性好,灵敏姓高,等特点。
附图说明
图1为原油中十八烷基二甲基甜菜碱的浓度-色谱峰面积之间的线性关系。
图2 为原油中200 mg/L十八烷基二甲基甜菜碱的质谱色谱图。
具体实施方式
下面通过具体实施例对本发明原油中十八烷基二甲基甜菜碱的液相色谱分析检测方法作进一步说明。
实施例一
1、待测样品配制
取3种待检测原油样品6AT235、6AT216、6A237 各2 mL,分别用2 mL正己烷稀释,混匀,然后,用4 mL乙醇/水混合液萃取原油/正己烷混合液中的甜菜碱表面活性剂,静置分层,取乙醇/水萃取液,20 µL进样。
2、检测
实施例二
1、样品配制
往6AT235、6AT216、6A237三种原油分别添加100 mg/L的十八烷基二甲基甜菜碱,分别取上述加标原油样品2 mL,用2 mL正己烷稀释,混匀,然后,用4 mL乙醇/水混合液萃取原油/正己烷混合液中的加标甜菜碱表面活性剂,静置分层,取乙醇/水萃取液,20 µL进样。
2、检测
Claims (2)
1.液相色谱分析检测原油中十八烷基二甲基甜菜碱的方法,包括以下内容:
(1)待测原油样品前处理
将待检测原油样品与正己烷以1:1的体积比混匀,得到原油/正己烷混合液;再采用体积比1:1的乙醇/水混合液萃取上述原油/正己烷混合液中的甜菜碱表面活性剂,静置分层,萃取液作为进样样品;
(2)色谱条件
色谱柱:25 cm C18色谱柱;
流动相:乙腈/水的混合液,体积比3/2,流速1.0 mL/min;
检测器:质谱检测器,ESI源,正模式检测;
(3)外标法定量
将经步骤(1)前处理的待测样品在上述色谱条件下进样,进样量20 μL,测定十八烷基二甲基甜菜碱的峰面积,依据线性关系计算原油样品中十八烷基二甲基甜菜碱的浓度;在50~500 mg/L范围内,原油中十八烷基二甲基甜菜碱的浓度与色谱峰面积之间具有良好的线性关系,具体线性方程为:
Y = 98992000 + 9638310 X,线性相关系数R = 0.99968;
其中,X——十八烷基二甲基甜菜碱的浓度,单位mg/L;
Y——质谱色谱峰面积,单位:Intens。
2.如权利要求1所述液相色谱分析检测原油中十八烷基二甲基甜菜碱的方法,其特征在于:所述乙醇/水混合液与原油/正己烷混合液的体积比为1:1。
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Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103940931A (zh) * | 2014-05-08 | 2014-07-23 | 山东省化工研究院 | 一种甜菜碱饲料添加剂质量综合评估方法 |
CN105067741A (zh) * | 2015-07-30 | 2015-11-18 | 宁夏泰瑞制药股份有限公司 | 一种甜菜碱含量的测定方法 |
CN106324164A (zh) * | 2015-06-30 | 2017-01-11 | 天津市药品检验所 | 一种枸杞子配方颗粒中甜菜碱含量测定的方法 |
CN107632097A (zh) * | 2017-09-14 | 2018-01-26 | 上海上药第生化药业有限公司 | 甜菜碱和肉碱的分离方法及其应用 |
CN108593798A (zh) * | 2018-04-26 | 2018-09-28 | 中国科学院兰州化学物理研究所 | 高效液相色谱测定油井注采液中磺基甜菜碱表活剂含量的方法 |
CN110771767A (zh) * | 2019-11-01 | 2020-02-11 | 陕西师范大学 | 一种缓解视疲劳枸杞叶固体饮料及其制备方法 |
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Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103940931A (zh) * | 2014-05-08 | 2014-07-23 | 山东省化工研究院 | 一种甜菜碱饲料添加剂质量综合评估方法 |
CN106324164A (zh) * | 2015-06-30 | 2017-01-11 | 天津市药品检验所 | 一种枸杞子配方颗粒中甜菜碱含量测定的方法 |
CN105067741A (zh) * | 2015-07-30 | 2015-11-18 | 宁夏泰瑞制药股份有限公司 | 一种甜菜碱含量的测定方法 |
CN107632097A (zh) * | 2017-09-14 | 2018-01-26 | 上海上药第生化药业有限公司 | 甜菜碱和肉碱的分离方法及其应用 |
CN108593798A (zh) * | 2018-04-26 | 2018-09-28 | 中国科学院兰州化学物理研究所 | 高效液相色谱测定油井注采液中磺基甜菜碱表活剂含量的方法 |
CN110771767A (zh) * | 2019-11-01 | 2020-02-11 | 陕西师范大学 | 一种缓解视疲劳枸杞叶固体饮料及其制备方法 |
Non-Patent Citations (1)
Title |
---|
三元采出液中磺基甜菜碱分析方法研究;张灿;《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》;20180215(第02期);摘要,第4.2.3-4.2.7节 * |
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