波长色散X射线荧光光谱法测定磷酸酯抗燃油中氯含量
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摘要
建立了基于波长色散X射线荧光光谱法(WD-XRF)测定磷酸酯抗燃油中的氯含量的方法,研究了抗燃油中水分、酸值、矿物油等杂质对测试结果的影响。校准曲线的相关系数为0. 9993,水分和酸值对测试结果基本没有影响,矿物油有稀释作用。方法评价表明检出限为1. 3 mg/kg,定量限为4. 3 mg/kg,相对标准偏差小于5%,回收率为95. 1%～104. 8%。方法已应用于检测近百台次抗燃油中的氯含量,有力支撑了电液调节系统的安全稳定运行。
The method for determination of chlorine content in phosphate ester based fire-resistant hydraulic fluid via wavelength dispersion X-ray fluorescence spectrometry was established. The influences of water content, acid value and mineral oil in fire-resistant hydraulic fluid were investigated. The correlation coefficient of calibration curve was 0. 9993. Water content and acid value have no effect while mineral oil has dilution effect on the results. Method evaluation indicated that the limit of detection is 1. 3 mg/kg,the limit of quantitation is 4. 3 mg/kg,the relative standard deviation is lower than 5%,and the recoveries are between 95. 1% and 104. 8%. This method has been applied to determine nearly one hundred of fire-resistant hydraulic fluid samples.
The method for determination of chlorine content in phosphate ester based fire-resistant hydraulic fluid via wavelength dispersion X-ray fluorescence spectrometry was established. The influences of water content, acid value and mineral oil in fire-resistant hydraulic fluid were investigated. The correlation coefficient of calibration curve was 0. 9993. Water content and acid value have no effect while mineral oil has dilution effect on the results. Method evaluation indicated that the limit of detection is 1. 3 mg/kg,the limit of quantitation is 4. 3 mg/kg,the relative standard deviation is lower than 5%,and the recoveries are between 95. 1% and 104. 8%. This method has been applied to determine nearly one hundred of fire-resistant hydraulic fluid samples.
引文
[1] Su J M,Meng Y C,Liu Y L. Oil analysis and management in electric power industry. Beijing:China Power Press,2009:112孙坚明,孟玉婵,刘永洛.电力用油分析及油务管理.北京:中国电力出版社,2009:112
[2] Zhao M Q,Lei A L. Corrosion and protection of metal,Beijing:National Defense Industry Press,2011:215赵麦群,雷阿丽,金属的腐蚀与防护.北京:国防工业出版社,2011:215
[3] Liu K,Xu S,He T X,Feng B. Electric Power Construction,2013,34(8):87刘凯,徐松,何铁祥,冯兵.电力建设,2013,34(8):87
[4] DL/T 571-2014Guidelines for the operation and maintenance of phosphate resistant fuel for power plants.DL/T 571-2014电厂用磷酸酯抗燃油运行维护导则
[5] DL/T 433-2015Determination of chlorine content in fire-resistant hydraulic fluid(bomb method).DL/T 433-2015抗燃油中氯含量测定方法-氧弹法
[6] Ming J L,Pan Y Z,Zhou F M. Thermal Power Generation,2011,40(8):30明菊兰,潘瑛芝,周飞梅.热力发电,2011,40(8):30
[7] Zhai L,Zhan X C,Chin. J. Anal. Lab.,2015,34(4):484翟磊,詹秀春.分析试验室,2015,34(4):484
[8] Tian M J,Zhou H M,Min H,Lin M. Chin. J. Anal. Lab.,2013,32(12):22田旻洁,周海明,闵红,林苗.分析试验室,2013,32(12):22
[9] Domingos E,Pereira T M C,Filgueiras P R. X-ray. Spectrom.,2013,42(2):79
[10] Ji A,Tao G Y,Zhuo S J,Luo L Q,X ray fluorescence spectroscopy,Beijing:Science Press,2003:1吉昂,陶光仪,卓尚军,罗立强. X射线荧光光谱分析.北京:科学出版社,2003:1
[11] Wang G X,Hu Y,Luo Q,Li D,Chen C,Lai W C,Zhai J,Chin. J. Anal. Lab.,2017,36(6):663王广西,胡燕,罗琼,李丹,陈诚,赖万昌,翟娟.分析试验室,2017,36(6):663
[12] Lai M S,Xiang L W,Lin J M,Li H F. Sci. China. Chem.,2013,56(8):1164
[13] Gazulla M F,Rodrigo M,Vicente S. X-Ray. Spectrom.,2010,39(5):321
[14] ISO 15597-2001Petroleum and related products-determination of chlorine and bromine content-wavelength-dispersive xray fluorescence spectrometry method ISO 15597-2001波长色散X射线荧光光谱法测定石油和相关产品中氯和溴的标准实验方法
[2] Zhao M Q,Lei A L. Corrosion and protection of metal,Beijing:National Defense Industry Press,2011:215赵麦群,雷阿丽,金属的腐蚀与防护.北京:国防工业出版社,2011:215
[3] Liu K,Xu S,He T X,Feng B. Electric Power Construction,2013,34(8):87刘凯,徐松,何铁祥,冯兵.电力建设,2013,34(8):87
[4] DL/T 571-2014Guidelines for the operation and maintenance of phosphate resistant fuel for power plants.DL/T 571-2014电厂用磷酸酯抗燃油运行维护导则
[5] DL/T 433-2015Determination of chlorine content in fire-resistant hydraulic fluid(bomb method).DL/T 433-2015抗燃油中氯含量测定方法-氧弹法
[6] Ming J L,Pan Y Z,Zhou F M. Thermal Power Generation,2011,40(8):30明菊兰,潘瑛芝,周飞梅.热力发电,2011,40(8):30
[7] Zhai L,Zhan X C,Chin. J. Anal. Lab.,2015,34(4):484翟磊,詹秀春.分析试验室,2015,34(4):484
[8] Tian M J,Zhou H M,Min H,Lin M. Chin. J. Anal. Lab.,2013,32(12):22田旻洁,周海明,闵红,林苗.分析试验室,2013,32(12):22
[9] Domingos E,Pereira T M C,Filgueiras P R. X-ray. Spectrom.,2013,42(2):79
[10] Ji A,Tao G Y,Zhuo S J,Luo L Q,X ray fluorescence spectroscopy,Beijing:Science Press,2003:1吉昂,陶光仪,卓尚军,罗立强. X射线荧光光谱分析.北京:科学出版社,2003:1
[11] Wang G X,Hu Y,Luo Q,Li D,Chen C,Lai W C,Zhai J,Chin. J. Anal. Lab.,2017,36(6):663王广西,胡燕,罗琼,李丹,陈诚,赖万昌,翟娟.分析试验室,2017,36(6):663
[12] Lai M S,Xiang L W,Lin J M,Li H F. Sci. China. Chem.,2013,56(8):1164
[13] Gazulla M F,Rodrigo M,Vicente S. X-Ray. Spectrom.,2010,39(5):321
[14] ISO 15597-2001Petroleum and related products-determination of chlorine and bromine content-wavelength-dispersive xray fluorescence spectrometry method ISO 15597-2001波长色散X射线荧光光谱法测定石油和相关产品中氯和溴的标准实验方法