CN102338786A - 变压器油中钝化剂的高效液相色谱检测方法 - Google Patents

变压器油中钝化剂的高效液相色谱检测方法 Download PDF

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CN102338786A
CN102338786A CN2010102357602A CN201010235760A CN102338786A CN 102338786 A CN102338786 A CN 102338786A CN 2010102357602 A CN2010102357602 A CN 2010102357602A CN 201010235760 A CN201010235760 A CN 201010235760A CN 102338786 A CN102338786 A CN 102338786A
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transformer oil
passivant
passivator
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朱向群
龚秋霖
厉敏宪
彭伟
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East China Power Test and Research Institute Co Ltd
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Abstract

本发明提供一种变压器油中钝化剂的高效液相色谱检测方法，采用高效液相色谱仪进行检测，选择长度为150～250mm，柱径为4.6mm的色谱柱，其中填料为硅，粒径为5um，孔径为

Description

变压器油中钝化剂的高效液相色谱检测方法
技术领域
本发明涉及一种变压器油中钝化剂的高效液相色谱检测方法。
背景技术
近年来，许多国家的变压器和电抗器出现与变压器油中腐蚀性硫有关的故障。变压器油中的腐蚀性硫与铜导体反应生成硫化亚铜沉积物，是造成这类故障的原因。在油中添加钝化剂是防止硫化亚铜沉积风险的一种方法，可有效地在裸露金属导线表面形成保护膜，减少铜离子与硫的化学反应，阻止变压器油产生硫腐蚀，从而杜绝由此诱发的绝缘事故。目前已有较多公司在变压器油中添加了一种Irgamet 39TM钝化剂，但对于添加后的钝化剂在油中的变化情况尚未掌握，原因是国内外没有建立绝缘油中irgamet 39TM钝化剂含量的检测方法。
发明内容
本发明要解决技术问题是提供变压器油中钝化剂的高效液相色谱检测方法，为确定添加后的钝化剂在油中的变化趋势，测定变压器油中钝化剂含量，以达到对添加钝化剂后的变压器油进行监测和调整，防止硫化亚铜沉积及硫腐蚀的发生。
本发明的变压器油中钝化剂的高效液相色谱检测方法，采用高效液相色谱仪，选择长度为150～250mm，柱径为4.6mm的色谱柱，其中填料为硅，粒径为5um，孔径为
Figure BSA00000203564600011
进样量10～20微升，流量1毫升/分钟，柱温30～35℃，流动相为甲醇水溶液，检测器为紫外吸收检测器。
所述流动相中甲醇和水的体积比为70∶30～60∶40。
所述色谱柱可以是C8色谱柱，色谱柱的长度为250mm；也可以是C18色谱柱，色谱柱的长度为150mm。
所述钝化剂优选为苯并三氮唑衍生物，其物理性质如下：外观透明，黄到棕色液体，粘度80mm2/s，密度(20℃)0.95g/cm3，闪点＞150℃(COC)，水＜0.01％，矿物油＞5％，氮含量14.6％。例如Ciba Specialty Chemicals公司提供的Irgamet39TM钝化剂。
本方法采用高效液相色谱(HPLC)检测技术进行测定，特别适用于对苯并三氮唑衍生物类钝化剂在变压器油中含量的测定。通过高效液相色谱中色谱柱、流动相及比例、流量、柱温以及进样量的选择，实现对变压器油中添加的Irgamet39TM钝化剂的定量测定。采用本方法可有效检测变压器油中添加的Irgamet39TM钝化剂含量以及变化趋势，以期达到调整和监控钝化剂浓度水平，防止变压器硫腐蚀。
附图说明
图1为实施例1检测结果的色谱图。
图2为标准曲线图。
具体实施方式
实施例1
采用waters高效液相色谱仪对含Irgamet39TM钝化剂浓度分别为10、50、100、150、200毫克/升的变压器油样品进行检测，选择Symmetry C8色谱柱，色谱柱的长度250mm，柱径为4.6mm，填料为硅，粒径为5um，孔径为
Figure BSA00000203564600021
进样量10微升，流量1毫升/分钟，柱温35℃，流动相为甲醇水溶液(甲醇和水的体积比为70∶30)，检测器为Waters CapLC 2487紫外可见双波长检测器。检测结果如图1所示，在4.05min处有钝化剂(Irgamet 39)检测峰。典型的色谱图见图1。采用标准曲线外标法(图2)进行定量检测。通过应用该方法可准确检测变压器油中钝化剂Irgamet39TM含量。
实施例2
采用waters高效液相色谱仪对含有Irgamet39TM钝化剂的变压器油进行检测，选择Symmetry C18色谱柱，色谱柱的长度为150mm，柱径为4.6mm，填料为硅，粒径为5um，孔径为进样量20微升，流量1毫升/分钟，柱温30℃，流动相为甲醇水溶液(甲醇和水的体积比为60∶40)，检测器为Waters CapLC2487紫外可见双波长检测器。

Claims (5)

1.变压器油中钝化剂的高效液相色谱检测方法，采用高效液相色谱仪进行检测，其特征在于，选择长度为150～250mm，柱径为4.6mm的色谱柱，其中填料为硅，粒径为5um，孔径为进样量10～20微升，流量1毫升/分钟，柱温30～35℃，流动相为甲醇水溶液，检测器为紫外吸收检测器。
2.如权利要求1所述的检测方法，其特征在于，所述流动相中甲醇和水的体积比为70∶30～60∶40。
3.如权利要求1所述的检测方法，其特征在于，所述色谱柱的长度为250mm。
4.如权利要求1所述的检测方法，其特征在于，所述色谱柱的长度为150mm。
5.如权利要求1～4任一项所述的检测方法，其特征在于，所述钝化剂为苯并三氮唑衍生物。
CN2010102357602A 2010-07-23 2010-07-23 变压器油中钝化剂的高效液相色谱检测方法 Pending CN102338786A (zh)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103267768A (zh) * 2013-01-15 2013-08-28 长沙理工大学 可用于变压器故障诊断的混合相油核磁共振分析方法
CN104007192A (zh) * 2014-05-08 2014-08-27 广东电网公司电力科学研究院 绝缘油中金属钝化剂、糠醛和抗氧化剂的测定方法
CN115144503A (zh) * 2022-07-06 2022-10-04 沈阳防锈包装材料有限责任公司 一种气相防锈膜中苯甲酸和苯并三氮唑含量的测定方法

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20090001330A1 (en) * 2007-06-28 2009-01-01 Chevron U.S.A. Inc. Electrical Insulating Oil Compositions and Preparation Thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20090001330A1 (en) * 2007-06-28 2009-01-01 Chevron U.S.A. Inc. Electrical Insulating Oil Compositions and Preparation Thereof
CN101688147A (zh) * 2007-06-28 2010-03-31 雪佛龙美国公司 电绝缘油组合物及其制备方法

Non-Patent Citations (7)

* Cited by examiner, † Cited by third party
Title
DUVAL M等: "《Dielectric behavior and stabilization of insulating oils in EHV current transformers》", 《ELECTRICAL INSULATION》 *
INTERNATIONAL ELECTROTECHNICAL COMMISSION: "《International Standard IEC-60666 Detection and determination of specified additives in mineral insulating oils》", 30 April 2010 *
YASUDA M等: "Suppression of static electrification of insulating oil for large power transformer", 《1982 IEEE PES WINTER MEETING》 *
唐鹏武: "苯并三氮唑及其衍生物的合成研究", 《中国优秀硕士学位论文全文数据库工程科技I辑》 *
连鸿松等: "变压器绝缘油硫腐蚀原因与对策", 《福建电力与电工》 *
陆志浩等: "大型变压器绝缘油中硫腐蚀的危害及防护对策研究", 《华东电力》 *
陈丽华等: "金属减活剂改善变压器油使用性能的探讨", 《石油学报(石油加工)》 *

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103267768A (zh) * 2013-01-15 2013-08-28 长沙理工大学 可用于变压器故障诊断的混合相油核磁共振分析方法
CN104007192A (zh) * 2014-05-08 2014-08-27 广东电网公司电力科学研究院 绝缘油中金属钝化剂、糠醛和抗氧化剂的测定方法
CN115144503A (zh) * 2022-07-06 2022-10-04 沈阳防锈包装材料有限责任公司 一种气相防锈膜中苯甲酸和苯并三氮唑含量的测定方法
CN115144503B (zh) * 2022-07-06 2024-05-24 沈阳防锈包装材料有限责任公司 一种气相防锈膜中苯甲酸和苯并三氮唑含量的测定方法

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