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Article(id=1209857949661524211, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1209857942514438502, articleNumber=null, orderNo=null, doi=10.16790/j.cnki.1009-9239.im.2022.02.016, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=research-article, receivedDate=1618329600000, receivedDateStr=2021-04-14, revisedDate=1621785600000, revisedDateStr=2021-05-24, acceptedDate=null, acceptedDateStr=null, onlineDate=1766382213273, onlineDateStr=2025-12-22, pubDate=1645286400000, pubDateStr=2022-02-20, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1766382213273, onlineIssueDateStr=2025-12-22, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1766382213273, creator=13701087609, updateTime=1766382213273, updator=13701087609, issue=Issue{id=1209857942514438502, tenantId=1146029695717560320, journalId=1149653034449285133, year='2022', volume='55', issue='2', pageStart='1', pageEnd='127', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1766382211568, creator=13701087609, updateTime=1766562990768, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1210616185499021709, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1209857942514438502, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1210616185499021710, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1209857942514438502, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=111, endPage=117, ext={EN=ArticleExt(id=1209857949980291330, articleId=1209857949661524211, tenantId=1146029695717560320, journalId=1149653034449285133, language=EN, title=Determination of Fatty Acid Content in Natural Ester Insulating Oil by 1H-NMR Spectroscopy, columnId=1192878364340924664, journalTitle=Insulating Materials, columnName=Test and Analysis, runingTitle=null, highlight=null, articleAbstract=

Natural ester insulating oil is a kind of environmentally-friendly liquid dielectrics with good insulation properties, and it has been generally applied in oil-filled electrical equipment. Investigating the types and contents of fatty acids in different natural ester insulating oils will be beneficial to grasp the physical and chemical properties of different insulating oils. In this paper, a method of determining the fatty acid composition in natural ester by 1H-NMR was presented, and the results were compared with that of GC-MS. The results show that this simple and rapid determination of fatty acid content in natural ester insulating oil by 1H-NMR is feasible and reliable. The maximum error absolute value of fatty acids content measured by 1H-NMR spectroscopy and GC-MS is 2.95%, which is in the tolerance interval.

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天然酯绝缘油作为一种新型难燃环保型液体绝缘介质，在液浸式电力设备中的应用越来越广泛，研究不同天然酯绝缘油的脂肪酸种类和含量，有利于掌握不同绝缘油的理化性能。本研究提出通过核磁共振氢谱法测定天然酯绝缘油脂肪酸组成的方法，并将其结果与气相色谱-质谱联用技术的测试结果进行比较。结果表明：利用核磁共振氢谱法对天然酯绝缘油的脂肪酸含量进行简单、快速的测定是可行且可靠的。核磁共振氢谱法与气相色谱-质谱法测定脂肪酸的误差绝对值最大为2.95%，该误差在可接受范围内。

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宋浩永（1985-），男（汉族），河南许昌人，高级工程师，主要从事绿色绝缘材料的研发及应用的研究。

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宋浩永（1985-），男（汉族），河南许昌人，高级工程师，主要从事绿色绝缘材料的研发及应用的研究。

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宋浩永（1985-），男（汉族），河南许昌人，高级工程师，主要从事绿色绝缘材料的研发及应用的研究。

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Bioresource Technology,2011,102(15):7280-7288., articleTitle=Multiple response optimization of vegetable oils fatty acid composition to improve bio-diesel physical properties, refAbstract=null)], funds=[Fund(id=1211015297138561435, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1209857949661524211, awardId=GZHKJXM20170063, language=CN, fundingSource=南方电网公司科技项目(GZHKJXM20170063), fundOrder=null, country=null)], companyList=[AuthorCompany(id=1211015292881342777, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1209857949661524211, xref=null, ext=[AuthorCompanyExt(id=1211015292893925690, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1209857949661524211, companyId=1211015292881342777, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=Guangzhou Power Supply Bureau of Guangdong Power Grid Corporation, Guangzhou 510000, China), AuthorCompanyExt(id=1211015292902314299, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1209857949661524211, companyId=1211015292881342777, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=广东电网有限责任公司广州供电局，广东 广州 510000)])], figs=[ArticleFig(id=1211015295695720812, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1209857949661524211, language=EN, label=Fig.1, caption=Assignment of signals of glycerol units and fatty acid chains, figureFileSmall=ECK5flC4tAwkTxdX8ehuNA==, figureFileBig=vLvX/A84F0JtDKblHwIVtA==, tableContent=null), ArticleFig(id=1211015295758635373, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1209857949661524211, language=CN, label=图1, caption=甘油单元和脂肪酸链的信号归属, figureFileSmall=ECK5flC4tAwkTxdX8ehuNA==, figureFileBig=vLvX/A84F0JtDKblHwIVtA==, tableContent=null), ArticleFig(id=1211015295855104366, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1209857949661524211, language=EN, label=Fig.2, caption=1H-NMR spectra of natural ester insulating oil, figureFileSmall=RJnxoWGcGc1211ofk/TUrg==, figureFileBig=tihrVpMrxfayoagiyih5Ow==, tableContent=null), ArticleFig(id=1211015295922213231, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1209857949661524211, language=CN, label=图2, caption=天然酯绝缘油的1H-NMR谱图, figureFileSmall=RJnxoWGcGc1211ofk/TUrg==, figureFileBig=tihrVpMrxfayoagiyih5Ow==, tableContent=null), ArticleFig(id=1211015295976739187, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1209857949661524211, language=EN, label=Tab.1, caption=Fundamental physical and chemical properties of three types of natural ester insulating oil, figureFileSmall=null, figureFileBig=null, tableContent=
指标大豆基天然酯绝缘油菜籽基天然酯绝缘油山茶籽基天然酯绝缘油标准限值
运动黏度(40℃)/(mm2/s)33.635.839.9≤50
酸值/(mg KOH/g)0.030.040.04≤0.06
燃点/℃360360341≥300
开口闪点/℃330322312≥250
倾点/℃-21-20-19≤-10
密度(20℃)/(g/cm3)0.9240.9170.910≤1
), ArticleFig(id=1211015296052236662, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1209857949661524211, language=CN, label=表1, caption=

3种天然酯绝缘油的基本理化性能

, figureFileSmall=null, figureFileBig=null, tableContent=
指标大豆基天然酯绝缘油菜籽基天然酯绝缘油山茶籽基天然酯绝缘油标准限值
运动黏度(40℃)/(mm2/s)33.635.839.9≤50
酸值/(mg KOH/g)0.030.040.04≤0.06
燃点/℃360360341≥300
开口闪点/℃330322312≥250
倾点/℃-21-20-19≤-10
密度(20℃)/(g/cm3)0.9240.9170.910≤1
), ArticleFig(id=1211015296115151224, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1209857949661524211, language=EN, label=Tab.2, caption=Assignment of peaks in 1H-NMR of natural ester insulating oil, figureFileSmall=null, figureFileBig=null, tableContent=
编号化学位移/(×10-6)氢核质子基团归属
A0.75～0.95-CH3饱和脂肪酸、单烯酸、二烯酸末端甲基上的H
B0.95～1.03-CH3三烯酸末端的H
C1.10～1.52-(CH2)n-烷基链的H
D1.52～1.70-OCO-CH2-CH2-羰基β位质子氢
E1.90～2.24-CH2-CH=CH-不饱和脂肪酸中与C=C双键相邻的亚甲基的H
F2.24～2.50-OCO-CH2-羰基α位质子氢
G2.60～2.96=HC-CH2-CH=

多不饱和脂肪酸上位于2个

C=C双键之间的亚甲基的H

H4.00～4.50-CH2OCOR甘油骨架上亚甲基的H
I5.23～5.30>CHOCOR甘油骨架上次甲基的H
J5.30～5.60-CH=CH-所有不饱和脂肪酸中双键上的H
), ArticleFig(id=1211015296199037308, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1209857949661524211, language=CN, label=表2, caption=

天然酯绝缘油核磁共振氢谱中各峰的归属

, figureFileSmall=null, figureFileBig=null, tableContent=
编号化学位移/(×10-6)氢核质子基团归属
A0.75～0.95-CH3饱和脂肪酸、单烯酸、二烯酸末端甲基上的H
B0.95～1.03-CH3三烯酸末端的H
C1.10～1.52-(CH2)n-烷基链的H
D1.52～1.70-OCO-CH2-CH2-羰基β位质子氢
E1.90～2.24-CH2-CH=CH-不饱和脂肪酸中与C=C双键相邻的亚甲基的H
F2.24～2.50-OCO-CH2-羰基α位质子氢
G2.60～2.96=HC-CH2-CH=

多不饱和脂肪酸上位于2个

C=C双键之间的亚甲基的H

H4.00～4.50-CH2OCOR甘油骨架上亚甲基的H
I5.23～5.30>CHOCOR甘油骨架上次甲基的H
J5.30～5.60-CH=CH-所有不饱和脂肪酸中双键上的H
), ArticleFig(id=1211015296257757568, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1209857949661524211, language=EN, label=Tab.3, caption=Contents of fatty acid methyl esters in natural ester insulating oils and molecular structure properties, figureFileSmall=null, figureFileBig=null, tableContent=
脂肪酸甲酯分子式大豆基天然酯绝缘油菜籽基天然酯绝缘油山茶籽基天然酯绝缘油
棕榈酸甲酯C17:0/%C17H34O210.605.5011.55
硬脂酸甲酯C19:0/%C19H38O25.192.563.64
油酸甲酯C19:1/%C19H36O226.6658.2360.67
亚油酸甲酯C19:2/%C19H34O248.1020.3520.41
亚麻酸甲酯C19:3/%C19H32O27.8610.422.75
花生酸甲酯C21:0/%C21H42O20.590.830.17
二十烯酸甲酯C21:1/%C21H40O20.301.650.68
二十二酸甲酯C23:0/%C23H46O20.700.460.14
不饱和脂肪酸/%—82.9290.6684.50
链长1—17.8317.9617.79
不饱和度2—1.461.301.10
分子量3—874.22880.32874.63
), ArticleFig(id=1211015296329060738, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1209857949661524211, language=CN, label=表3, caption=

天然酯绝缘油中各脂肪酸甲酯的含量及其分子结构性质

, figureFileSmall=null, figureFileBig=null, tableContent=
脂肪酸甲酯分子式大豆基天然酯绝缘油菜籽基天然酯绝缘油山茶籽基天然酯绝缘油
棕榈酸甲酯C17:0/%C17H34O210.605.5011.55
硬脂酸甲酯C19:0/%C19H38O25.192.563.64
油酸甲酯C19:1/%C19H36O226.6658.2360.67
亚油酸甲酯C19:2/%C19H34O248.1020.3520.41
亚麻酸甲酯C19:3/%C19H32O27.8610.422.75
花生酸甲酯C21:0/%C21H42O20.590.830.17
二十烯酸甲酯C21:1/%C21H40O20.301.650.68
二十二酸甲酯C23:0/%C23H46O20.700.460.14
不饱和脂肪酸/%—82.9290.6684.50
链长1—17.8317.9617.79
不饱和度2—1.461.301.10
分子量3—874.22880.32874.63
), ArticleFig(id=1211015296387780996, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1209857949661524211, language=EN, label=Tab.4, caption=Contents of fatty acid methyl esters by 1H-NMR, figureFileSmall=null, figureFileBig=null, tableContent=
脂肪酸种类质量分数/%
大豆基天然酯绝缘油菜籽基天然酯绝缘油山茶籽基天然酯绝缘油
三烯酸7.449.462.73
二烯酸49.7218.6717.45
单烯酸26.0762.4962.97
饱和脂肪酸16.779.3816.85
), ArticleFig(id=1211015296463278472, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1209857949661524211, language=CN, label=表4, caption=

1H-NMR测得脂肪酸甲酯的含量

, figureFileSmall=null, figureFileBig=null, tableContent=
脂肪酸种类质量分数/%
大豆基天然酯绝缘油菜籽基天然酯绝缘油山茶籽基天然酯绝缘油
三烯酸7.449.462.73
二烯酸49.7218.6717.45
单烯酸26.0762.4962.97
饱和脂肪酸16.779.3816.85
), ArticleFig(id=1211015296538775946, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1209857949661524211, language=EN, label=Tab.5, caption=Contents of fatty acid in soybean-based natural ester insulating oil, figureFileSmall=null, figureFileBig=null, tableContent=
脂肪酸种类质量分数/%误差绝对值/%典型值/%
GC-MS测1H-NMR测
三烯酸7.867.440.427.81
二烯酸48.1049.721.6253.31
单烯酸26.9626.070.8923.45
饱和脂肪酸17.0816.770.3115.43
), ArticleFig(id=1211015296601690508, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1209857949661524211, language=CN, label=表5, caption=

大豆基天然酯绝缘油脂肪酸测定

, figureFileSmall=null, figureFileBig=null, tableContent=
脂肪酸种类质量分数/%误差绝对值/%典型值/%
GC-MS测1H-NMR测
三烯酸7.867.440.427.81
二烯酸48.1049.721.6253.31
单烯酸26.9626.070.8923.45
饱和脂肪酸17.0816.770.3115.43
), ArticleFig(id=1211015296681382288, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1209857949661524211, language=EN, label=Tab.6, caption=Contents of fatty acid in rapeseed-based natural ester insulating oil, figureFileSmall=null, figureFileBig=null, tableContent=
脂肪酸种类质量分数/%误差绝对值/%典型值/%
GC-MS测1H-NMR测
三烯酸10.429.460.968.15
二烯酸20.3518.671.6819.73
单烯酸59.8962.492.6063.51
饱和脂肪酸9.349.380.047.23
), ArticleFig(id=1211015296744296850, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1209857949661524211, language=CN, label=表6, caption=

菜籽基天然酯绝缘油脂肪酸测定

, figureFileSmall=null, figureFileBig=null, tableContent=
脂肪酸种类质量分数/%误差绝对值/%典型值/%
GC-MS测1H-NMR测
三烯酸10.429.460.968.15
二烯酸20.3518.671.6819.73
单烯酸59.8962.492.6063.51
饱和脂肪酸9.349.380.047.23
), ArticleFig(id=1211015296819794325, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1209857949661524211, language=EN, label=Tab.7, caption=Contents of fatty acid in camellia-based natural ester insulating oil, figureFileSmall=null, figureFileBig=null, tableContent=
脂肪酸种类质量分数/%误差绝对值/%
GC-MS测1H-NMR测
三烯酸2.752.730.02
二烯酸20.4117.452.95
单烯酸60.6762.971.62
饱和脂肪酸15.5016.851.35
), ArticleFig(id=1211015296895291800, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1209857949661524211, language=CN, label=表7, caption=

山茶籽基天然酯绝缘油脂肪酸测定

, figureFileSmall=null, figureFileBig=null, tableContent=
脂肪酸种类质量分数/%误差绝对值/%
GC-MS测1H-NMR测
三烯酸2.752.730.02
二烯酸20.4117.452.95
单烯酸60.6762.971.62
饱和脂肪酸15.5016.851.35
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核磁共振氢谱法测定天然酯绝缘油的脂肪酸含量
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宋浩永 , 王炜 , 黄青丹 , 莫文雄
绝缘材料 | 测试与分析 2022,55(2): 111-117
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绝缘材料 | 测试与分析 2022, 55(2): 111-117
核磁共振氢谱法测定天然酯绝缘油的脂肪酸含量
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宋浩永, 王炜, 黄青丹, 莫文雄
作者信息
  • 广东电网有限责任公司广州供电局，广东 广州 510000

    • 宋浩永（1985-），男（汉族），河南许昌人，高级工程师，主要从事绿色绝缘材料的研发及应用的研究。

Determination of Fatty Acid Content in Natural Ester Insulating Oil by 1H-NMR Spectroscopy
Haoyong SONG, Wei WANG, Qingdan HUANG, Wenxiong MO
Affiliations
  • Guangzhou Power Supply Bureau of Guangdong Power Grid Corporation, Guangzhou 510000, China
出版时间: 2022-02-20 doi: 10.16790/j.cnki.1009-9239.im.2022.02.016
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摘要
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天然酯绝缘油作为一种新型难燃环保型液体绝缘介质，在液浸式电力设备中的应用越来越广泛，研究不同天然酯绝缘油的脂肪酸种类和含量，有利于掌握不同绝缘油的理化性能。本研究提出通过核磁共振氢谱法测定天然酯绝缘油脂肪酸组成的方法，并将其结果与气相色谱-质谱联用技术的测试结果进行比较。结果表明：利用核磁共振氢谱法对天然酯绝缘油的脂肪酸含量进行简单、快速的测定是可行且可靠的。核磁共振氢谱法与气相色谱-质谱法测定脂肪酸的误差绝对值最大为2.95%，该误差在可接受范围内。

天然酯绝缘油  /  脂肪酸  /  核磁共振氢谱法  /  气相色谱-质谱法

Natural ester insulating oil is a kind of environmentally-friendly liquid dielectrics with good insulation properties, and it has been generally applied in oil-filled electrical equipment. Investigating the types and contents of fatty acids in different natural ester insulating oils will be beneficial to grasp the physical and chemical properties of different insulating oils. In this paper, a method of determining the fatty acid composition in natural ester by 1H-NMR was presented, and the results were compared with that of GC-MS. The results show that this simple and rapid determination of fatty acid content in natural ester insulating oil by 1H-NMR is feasible and reliable. The maximum error absolute value of fatty acids content measured by 1H-NMR spectroscopy and GC-MS is 2.95%, which is in the tolerance interval.

natural ester insulating oil  /  fatty acid composition  /  1H-NMR spectroscopy  /  GC-MS
宋浩永, 王炜, 黄青丹, 莫文雄. 核磁共振氢谱法测定天然酯绝缘油的脂肪酸含量. 绝缘材料, 2022 , 55 (2) : 111 -117 . DOI: 10.16790/j.cnki.1009-9239.im.2022.02.016
Haoyong SONG, Wei WANG, Qingdan HUANG, Wenxiong MO. Determination of Fatty Acid Content in Natural Ester Insulating Oil by 1H-NMR Spectroscopy[J]. Insulating Materials, 2022 , 55 (2) : 111 -117 . DOI: 10.16790/j.cnki.1009-9239.im.2022.02.016
正文
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0 引言
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天然酯绝缘油由大豆、油菜籽、葵花籽、棕榈果等植物基油料经过压榨或浸出、精炼、改性等工艺制备而成，是一种新型防火与环保的绝缘液体[1]。其28天的生物降解率可达97%，万一发生泄漏，不会对土壤和水源等造成环境污染[2]。在防火安全方面，天然酯绝缘油燃点高于300℃，属于K级难燃类绝缘材料，能有效减少火灾事故的发生[3]。天然酯绝缘油也具有良好的电气性能，其2.5 mm标准电极间距下的击穿电压可达到75 kV，介电常数约为矿物绝缘油的1.5倍[3]。除此之外，天然酯绝缘油能够延缓油纸绝缘中纤维素的热老化速率、延长油纸绝缘的寿命、提高电力设备的耐过负载能力[4-5]。基于这些优点，天然酯绝缘油在变压器等电力设备中的应用越来越广泛。
按照IEC 62770:2013的定义，天然酯绝缘油的主要成分为甘油三酸酯，不同天然酯绝缘油的主要区别在于甘油三酸酯上脂肪酸取代基的不同[6]。其中脂肪酸的种类有很多，通常其碳原子数为12～22，双键数为1～3。脂肪酸类型、含量的差异决定着天然酯绝缘油理化性能的不同。脂肪酸分子饱和程度越高，对应油品的氧化安定性越好；但油的倾点越高，低温流动性越差，油的黏度越大[4,7]。通过添加抗氧剂等添加剂可以使得绝缘油化学性能更稳定[8]，但是添加剂的含量一般保持在1%以下，以防止过量的添加导致绝缘油的电导率上升到不可接受的水平，因此天然酯绝缘油的氧化安定性、低温流动性等性质很大程度上仍取决于植物油本身。因此为了兼顾绝缘油的氧化安定性、低温流动性和散热性，在电力设备应用中选择最适合的天然酯绝缘油，有必要研究不同天然酯绝缘油的脂肪酸种类和含量。
ISO 12966:2017提出通过气相色谱法（GC）测定油脂中脂肪酸的类别和含量，这也是目前国内外最常用的脂肪酸测试方法[9]。它利用极性色谱柱分离不同碳链长度的脂肪酸，通过火焰离子化（FID）检测器进行定性定量分析。虽然气相色谱法具有检测不确定度小、检测结果重现性好的优点，但是这种方法预处理过程复杂，需要将脂肪酸甲酯化。不恰当的预处理方法和操作会导致样品的变化和污染，从而出现分析错误。除气相色谱法外，近年来利用气相色谱-质谱联用技术（GC-MS）［10-12]、高效液相色谱法（HPLC）[13]进行脂肪酸测定的研究也越来越多。还有学者利用红外光谱（IR）测定油脂的脂肪酸，该方法具有分析速度快、分析效率高、无污染、无需预处理、对样品无损伤等优点，但该方法建立在具有良好稳定性和强适应性的数学模型之上，需要收集大量有代表性的植物油样品，较为繁琐[14]。核磁共振（NMR）波谱被提出作为油脂脂肪酸含量分析的替代方法[15-16]。它是一种非破坏性、非侵入性的研究方法，无需在测定前进行繁琐的衍生化和预处理，通常只需要少量的样品以及有机溶剂，就能快速直接地对油脂的脂肪酸含量进行定性分析。目前核磁共振技术在食用油脂的检测分析方面有应用，例如鉴别食用油脂是否掺伪[17]、对食品或油料的含油量进行测定[18]以及为选种、育种、商检、质检提供新的手段[19]。
本研究提出采用核磁共振氢谱法（1H-NMR）测定天然酯绝缘油的脂肪酸含量，并和气相色谱-质谱（GC-MS）法的结果及绝缘油厂家提供的典型值进行对比，分析3种不同种类天然酯绝缘油的脂肪酸含量，并计算天然酯绝缘油中饱和脂肪酸和单烯酸、二烯酸、三烯酸不饱和脂肪酸的含量。
1 实验
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1.1 天然酯绝缘油的选取
选取大豆基、菜籽基、山茶籽基天然酯绝缘油，3种天然酯绝缘油的主要化学结构均为甘油三酸酯，其化学结构中脂肪酸类型与含量不同是导致绝缘油理化性能不同的主要原因之一。表1列举了这3种天然酯绝缘油的基本理化性能以及IEC 62770:2013给出的未使用天然酯绝缘油的理化性能限值。
从表1可以看出，3种天然酯绝缘油的燃点和开口闪点均超过300℃，属于K级难燃类绝缘材料。相对于矿物油40℃下的运动黏度（3～16 mm2/s），天然酯绝缘油的黏度均大于30 mm2/s，一定程度上会影响其散热能力。在低温流动性方面，天然酯绝缘油的倾点在-20℃左右，远高于矿物油的-45℃，因此一般会通过添加降凝剂的方法来改善天然酯绝缘油的低温性能[20]。
1.2 试剂与仪器
正庚烷、氘代氯仿，色谱纯；3%甲醇钠溶液、14%三氟化硼甲醇溶液、饱和氯化钠溶液、无水硫酸钠，分析纯，上海易恩化学技术有限公司。
气质联用仪，7890B-5977A型，安捷伦科技有限公司；核磁共振仪，AVANCE Ⅲ HD 600 MHz型，瑞士布鲁克公司。
1.3 气相色谱-质谱分析
参考ISO 12966-2:2017《Animal and vegetable fats and oils — Gas chromatography of fatty acid methyl esters》进行样品的甲酯化与气相色谱-质谱仪分析条件的设定[9]。
1.3.1 试样的预处理步骤
称取油样0.2 g置于100 mL三口烧瓶中。加入5～10 mL的3%甲醇钠溶液，将冷凝管固定于烧瓶上，水浴锅加热至（80±1）℃时，将烧瓶置于水浴中，加热回流直至油滴消失。用移液管从冷凝管顶部向烧瓶加入5～10 mL的14%三氟化硼甲醇溶液，在（80±1）℃水浴中继续回流反应5～10 min，使试剂甲酯化完全。用少量水冲洗回流冷凝器以减少冷凝管上甲酯化样品的残留。停止加热，从水浴上取下烧瓶，迅速冷却至室温。经三口烧瓶瓶口准确加入10 mL正庚烷，振摇2 min，静置分层后，加入饱和氯化钠溶液使得水层移动至烧瓶瓶颈的下端，吸取上层的正庚烷提取液5～25 mL于试管中。加入少量无水硫酸钠，振摇1 min，静置分层，吸取上层溶液到进样瓶中等待测定。
1.3.2 分析条件
选用VF-WAXms极性色谱柱（30 m×0.25 mm×0.25 μm），进样口温度设置为250℃，分流比设置为1∶30，进样量为1 μL，载气为99.999%高纯氦气，程序升温过程：初始温度为180℃，保持8 min，以10℃/min的速率升温至230℃，保持30 min。质谱部分扫描方式为SCAN扫描，离子源选择EI源，传输线为250℃，电离能量为70 eV，离子源温度为230℃，四极杆温度为150℃，扫描范围为35～500 m/z，溶剂延迟为2.5 min。
1.4 核磁共振氢谱分析
1.4.1 样品的预处理步骤
称取80 mg的绝缘油至5 mm的核磁共振样品管中，加入约0.6 mL氘代氯仿，将制好的样品充分振摇，进行核磁测定。
1.4.2 样品的1H-NMR谱图分析
能够用1H-NMR测定天然酯绝缘油的脂肪酸含量的关键原因是：天然酯绝缘油的主要成分为甘油三酸酯，它由甘油骨架和不同种类的脂肪酸构成，且其中不饱和脂肪酸主要成分包含单烯酸、二烯酸和三烯酸。甘油三酸酯中甘油骨架和脂肪酸上共存在有10种不同化学位移的氢核，本研究将其分别标注为A～J，如图1所示。这10种不同种类的氢核对应的化学位移不同，且1H-NMR信号峰面积的积分与对应氢核的数量成正比。因此通过归属甘油三酸酯中不同脂肪酸和甘油骨架氢核与1H-NMR谱图的对应关系，就能计算出不同脂肪酸的摩尔分数。天然酯绝缘油1H-NMR谱图中各信号峰的归属如表2所示。
1.4.3 脂肪酸含量的计算原理
样品1H-NMR谱图中的10个共振峰的峰面积与对应的氢核数量之间存在定量关系，因此可用于判断天然酯绝缘油中不同脂肪酸含量。
根据天然酯绝缘油1H-NMR谱图和各峰的归属可知，共振峰B只与三烯酸中的甲基氢有关，因此该峰面积积分值用于计算天然酯绝缘油中三烯酸的含量，其中天然酯绝缘油中的三烯酸均以亚麻酸的形式存在。因为与共振峰B相关的三烯酸甲基氢有3个，所以三烯酸的物质的量nTA可以通过测量信号峰B的面积得出。将信号峰A～J的面积积分值用AA～AJ表示，nTA与AB的关系如式（1）所示。
nTA=AB3
共振峰G处的信号是指两个C=C双键之间的亚甲基氢，只有二烯酸和三烯酸含有特征信号G，其中天然酯绝缘油中二烯酸均以亚油酸的形式存在。因为与共振峰G相关的三烯酸亚甲基氢有4个，二烯酸亚甲基氢有两个，所以二烯酸的物质的量nDA可以通过对信号峰G处的面积进行积分，再减去三烯酸提供的峰面积确定，即式（2）。
nDA=AG2-23AB
共振峰J由所有不饱和脂肪酸中双键上的氢产生，单烯酸、二烯酸和三烯酸都含有特征信号J，且与共振峰J相关的氢核，三烯酸含有6个，二烯酸含4个，单烯酸有两个，因此单烯酸的物质的量nMA可以通过计算峰J的面积积分值，并且结合nTA和nDA，通过式（3）计算得出。
nMA=13AB-AG+AJ2
共振峰A由二烯酸、单烯酸和饱和脂肪酸的甲基产生，在峰A的总面积中扣除不饱和脂肪酸相关的部分，即可用于计算饱和脂肪酸的物质的量nSaturated，即式（4）。
nSaturated=AA3+AB3+AG2-AJ2
ISO 12966测定动植物油脂脂肪酸含量的结果是用不同脂肪酸甲酯的质量分数来表示的，因此为了将核磁共振氢谱方法得到的测试结果与GC-MS方法比较，根据计算得到的不同种类脂肪酸物质的量和对应的相对分子质量，将天然酯绝缘油中脂肪酸的含量计算并表达为不同种类脂肪酸甲酯的质量分数。其中饱和脂肪酸的平均相对分子质量计算方法如下：天然酯绝缘油1H-NMR谱图中的共振峰C是由-(CH2)n-上的氢核产生的，利用共振峰C的积分值，结合已经计算得到的各不饱和脂肪酸物质的量和饱和脂肪酸物质的量，可以计算出图1所示饱和脂肪酸R1中(CH2)n的参数n值，如式（5）。从而确定饱和脂肪酸的链长为（n+4），进而可通过式（6）计算饱和脂肪酸甲酯的平均相对分子质量MSaturated。
n=(AC-20nMA-14nDA-8nTA)2nSaturated
MSaturated=14.03n+2+2×15.04+44.01
式（6）中：14.03、15.04和44.01分别代表饱和脂肪酸甲酯中的亚甲基、甲基和-OCO-酯基的摩尔质量。
2 结果与分析
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2.1 气相色谱-质谱分析
对甲酯化后的大豆基天然酯绝缘油、菜籽基天然酯绝缘油和山茶籽基天然酯绝缘油进行GC-MS分析，气相色谱将脂肪酸甲酯分离开，质谱结果与NIST质谱图检索库进行对比，确定脂肪酸甲酯的种类。采用面积归一化方法，依据不同脂肪酸甲酯各自的峰面积，定量分析出不同脂肪酸甲酯的相对质量分数，得到的3种天然酯绝缘油的脂肪酸甲酯含量如表3所示。
从表3可以看出，3种天然酯绝缘油中不饱和脂肪酸的含量均大于80%。大豆基天然酯绝缘油中亚油酸甲酯的含量最高，达到48.1%，菜籽基和山茶籽基天然酯绝缘油的油酸甲酯含量较多，达60%左右，菜籽基天然酯绝缘油的亚麻酸甲酯含量最高。计算得到大豆基、菜籽基、山茶籽基天然酯绝缘油的平均分子量分别为874.22、880.32、874.63。在三者化学结构相同、平均分子量相近的情况下，可以从微观分子角度得到天然酯绝缘油黏度、倾点等理化性能与不饱和度的关联。在不饱和脂肪酸中，碳碳双键的顺式结构导致绝缘油分子呈弯曲形，使得分子与分子之间无法紧密排列，导致其分子间的作用力减小，因此绝缘油的黏度和倾点会随着不饱和度的增加而减小。计算得到大豆基天然酯绝缘油含有更多的不饱和脂肪酸，其不饱和度为1.46，菜籽基绝缘油的不饱和度为1.30，山茶籽基绝缘油的不饱和度为1.10。因此，大豆基天然酯绝缘油的黏度和倾点小于菜籽基和山茶籽基天然酯。
2.2 核磁共振氢谱分析
利用核磁共振波谱仪测定的大豆基、菜籽基和山茶籽基天然酯绝缘油的1H-NMR谱图如图2所示。
为了验证1H-NMR谱图的正确性与消除核磁共振测量条件对峰强度的影响，因1个甘油骨架上含有4个亚甲基氢是恒定的，故在对谱图的每个共振峰进行积分后，将甘油骨架上的亚甲基氢的信号峰H峰面积归一化为4。发现共振峰I、F、D的面积分别为1、6、6，与甘油骨架上只有一个次甲基H、6个羰基α位质子氢、6个羰基β位质子氢完全一致，证明了1H-NMR谱图的准确性。根据脂肪酸含量计算原理，测定天然酯绝缘油中单烯酸、二烯酸、三烯酸和饱和脂肪酸的含量，具体结果如表4所示。与表3通过GC-MS方法测试出来的脂肪酸含量进行比较，结果误差均在可接受的范围内，说明利用核磁共振氢谱法测量天然酯绝缘油中单烯酸、二烯酸、三烯酸和饱和脂肪酸含量是可靠的。
3 讨论
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为了检验核磁共振氢谱法测定天然酯绝缘油脂肪酸组成方法的准确性，本研究不仅将其得到的结果与通过气相色谱-质谱法测定的结果进行比较，还收集了天然酯绝缘油生产厂家提供的脂肪酸含量的典型值作为参考，对比结果如表5～7所示。
从表5可以看出，对于大豆基天然酯绝缘油，1H-NMR法与GC-MS测得的饱和脂肪酸、单烯酸和三烯酸的含量误差绝对值均小于1%，二烯酸含量相差1.62%。从表6可以看出，对于菜籽基天然酯绝缘油，1H-NMR法与GC-MS测得单烯酸的含量误差最大为2.60%，仍符合误差要求。对于山茶籽基天然酯绝缘油，未收集到厂家提供的典型值，从表7可以看出，1H-NMR法与GC-MS法测定的二烯酸含量相差最大，但绝对误差仅为2.95%。最重要的是，与传统的气相色谱为标准的方法相比，核磁共振氢谱法不需要任何的样品预处理过程，不仅省时、省力、减少了化学品的消耗，而且避免了预处理过程偏差带来的分析错误。
4 结论
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本研究将核磁共振氢谱法应用于天然酯绝缘油的脂肪酸含量测试，将结果与通过气相色谱-质谱法测定结果相比，两者可以互相验证。大豆基天然酯中主要脂肪酸为二烯酸，两种方法测得二烯酸误差最大为1.62%；菜籽基天然酯和山茶籽基天然酯中主要脂肪酸为单烯酸，两种方法测得脂肪酸含量误差最大值分别为2.60%和2.95%，均符合误差要求。更重要的是，核磁共振氢谱法避免了气相色谱方法在测定之前需要繁琐的甲酯化预处理过程，只需要少量的样品与很短的时间，就能对天然酯绝缘油的脂肪酸含量进行定性分析，从而更快地掌握不同绝缘油理化性能变化的规律。此外还减少了化学品的消耗与废液的产生，从经济和环保角度也是有益的。综上，利用核磁共振氢谱法对天然酯绝缘油的脂肪酸含量进行简单、快速的测定是可行且可靠的。
基金
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  • 南方电网公司科技项目(GZHKJXM20170063)
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2022年第55卷第2期
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doi: 10.16790/j.cnki.1009-9239.im.2022.02.016
  • 接收时间：2021-04-14
  • 首发时间：2025-12-22
  • 出版时间：2022-02-20
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  • 收稿日期：2021-04-14
  • 修回日期：2021-05-24
基金
南方电网公司科技项目(GZHKJXM20170063)
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    广东电网有限责任公司广州供电局，广东 广州 510000
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鹅膏菌科Amanitaceae 2 11 5.26 鹅膏菌属 Amanita 10 4.78
小菇科 Mycenaceae 2 12 5.74 丝盖伞属 Inocybe 5 2.39
多孔菌科 Polyporaceae 8 14 6.70 蜡蘑属 Laccaria 5 2.39
红菇科 Russulaceae 3 23 11.00 小皮伞属 Marasmius 6 2.87
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红菇属 Russula 17 8.13
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