镍钛合金纤维/有机硅-聚氨酯固相微萃取头的制备及其在水中7种取代苯化合物检测中的应用
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摘要
以2,4-甲苯二异氰酸酯、聚酯多元醇、羟基硅油为原料,辛酸亚锡为催化剂,环己酮为溶剂,合成有机硅-聚酯型聚氨酯。将此聚合物涂于经氢氧化钾水热处理的镍钛合金纤维丝表面作为固相微萃取涂层,制得固相微萃取头。利用红外光谱法分析了聚合物结构;热重分析法确定了涂层最高使用温度;扫描电子显微镜观察了萃取头的表面形貌。以顶空萃取-固相微萃取-气相色谱法(HS-SPME-GC)测定了水中甲苯、二甲苯、间二氯苯、邻二氯苯、苯甲酸乙酯、硝基苯、苯甲醇7种取代苯化合物的含量。各被测物的色谱峰面积与其质量浓度呈良好的线性关系,相关系数(R2)为0. 992 6～0. 999 8,方法的检出限为0. 08～0. 24μg/L。实际样品测定的加标回收率为95. 9%～105. 4%,相对标准偏差为1. 4%～5. 0%。通过对实际样品的分析,说明制备的固相微萃取头涂层不易脱落、性质稳定,对于水中取代苯类化合物具有很强的吸附能力。
Toluene-2,4-diisocyanate,polyester polyol,and hydroxy silicone oil were used as raw materials;stannous octoate was used as the catalyst;and cyclohexanone was used as the solvent to synthesize organosilicone-polyurethane(SP). The polymer was coated on the surface of a nickel-titanium alloy fiber treated hydrothermally with potassium hydroxide. It was the prepared for headspace solid phase microextraction(HS-SPME). The polymer structure was analyzed by infrared spectroscopy,the highest temperature of the coating was determined by thermogravimetric analysis,and the surface morphology of the extraction head was observed by scanning electron microscopy. The benzene series of toluene,xylene,m-dichlorobenzene,odichlorobenzene,ethyl benzoate,nitrobenzene and benzyl alcohol in water were determined by HS-SPME-gas chromatography(GC)method. There was a good linear relationship between the chromatographic peak area and mass concentration of each measured object. The correlation coefficients(R2)were 0. 992 6-0. 999 8. The limits of detection were 0. 08-0. 24 μg/L. The recoveries of the spiked samples were 95. 9%-105. 4%,and the relative standard deviations were 1. 4%-5. 0%. The coating of SPME head adhered more firmly,and had a better adsorptionperformance for the substituted benzenes in water.
Toluene-2,4-diisocyanate,polyester polyol,and hydroxy silicone oil were used as raw materials;stannous octoate was used as the catalyst;and cyclohexanone was used as the solvent to synthesize organosilicone-polyurethane(SP). The polymer was coated on the surface of a nickel-titanium alloy fiber treated hydrothermally with potassium hydroxide. It was the prepared for headspace solid phase microextraction(HS-SPME). The polymer structure was analyzed by infrared spectroscopy,the highest temperature of the coating was determined by thermogravimetric analysis,and the surface morphology of the extraction head was observed by scanning electron microscopy. The benzene series of toluene,xylene,m-dichlorobenzene,odichlorobenzene,ethyl benzoate,nitrobenzene and benzyl alcohol in water were determined by HS-SPME-gas chromatography(GC)method. There was a good linear relationship between the chromatographic peak area and mass concentration of each measured object. The correlation coefficients(R2)were 0. 992 6-0. 999 8. The limits of detection were 0. 08-0. 24 μg/L. The recoveries of the spiked samples were 95. 9%-105. 4%,and the relative standard deviations were 1. 4%-5. 0%. The coating of SPME head adhered more firmly,and had a better adsorptionperformance for the substituted benzenes in water.
引文
[1] Xiao Q F,Dai X L,Wang X D,et al. Chinese Environmental Science,2005,25(1):18肖乾芬,戴玄吏,王晓栋,等.中国环境科学,2005,25(1):18
[2] Li X X,Liang X K,Feng G D,et al. Modern Instruments,2007,13(1):14李欣欣,梁学凯,冯国栋,等.现代仪器,2007,13(1):14
[3] Tumbiolo S,Gal J F,Maria P C,et al. Anal Chim,2005,95(11):757
[4] Duan G. Energy and Environment,2018(2):69段钢.能源与环境,2018(2):69
[5] Wang Y F,Shi J W,Wang L,et al. Chinese Journal of Chromatography,2015,33(4):451王玉飞,施家威,王立,等.色谱,2015,33(4):451
[6] Mei M,Huang X J. Chinese Journal of Chromatography,2016,34(12):1168梅萌,黄晓佳.色谱,2016,34(12):1168
[7] Fu R N. Chinese Journal of Analysis Laboratory,2015,34(5):602傅若农.分析试验室,2015,34(5):602
[8] Yang Y C,Hui Y Q,He X B,et al. Physical Testing and Chemical Analysis Part B:Chemical Analysis,2008,44(9):904杨宇川,辉永庆,何小波,等.理化检验:化学分册,2008,44(9):904
[9] Chen M,Yuan D X,Xu P X. Journal of Analytical Science,2002,18(5):429陈猛,袁东星,许鹏翔.分析科学学报,2002,18(5):429
[10] Ligor M,Scibiorek M,Buszewski B,et al. J Microcolumn Sep,2015,11(5):377
[11] Teresa C. J Wood Chem Tech,2014,34(3):211
[12] Chen N,Zhang Y J,Zhao W L,et al. Chinese Journal of Chromatography,2018,36(1):35陈娜,张毅军,赵万里,等.色谱,2018,36(1):35
[13] Gong T,Li F. Chemical Propellants&Polymeric Materials,2014,12(4):32宫涛,李汾.化学推进剂与高分子材料,2014,12(4):32
[14] Feng J J,Qiu H D,Liu X,et al. TrAC-Trends Anal Chem,2014,44(42):44
[15] Cao D D,Lv J X,Liu J F,et al. Anal Chim Acta,2008,611(1):56
[16] Liu H,Wang D,Ji L,et al. J Chromatogr A,2010,1217(12):1898
[17] Zeng J,Zhao C,Chong F,et al. J Chromatogr A,2013,1319(6):21
[18] Zeng J,Zhao C,Chen J,et al. J Chromatogr A,2014,1365:29
[19] Li Y,Ma M G,Zhang M,et al. Chinese Journal of Analysis Laboratory,2014,33(6):621李毅,马明广,张敏,等.分析试验室,2014,33(6):621
[20] Zhou S S,Jin P X,Wang Z Y,et al. Chinese Journal of Chromatography,2018,36(2):100周珊珊,金盼霞,王子宜,等.色谱,2018,36(2):100
[21] Es-Haghi A,Hosseini S M,Khoshhesab Z M. Anal Chim Acta,2012,742(17):74
[22] Du J J,Zhang M,Zhen Q,et al. Chinese Journal of Analytical Chemistry,2017,45(11):1662杜稼健,张敏,甄琦,等.分析化学,2017,45(11):1662
[23] Shen S C,Song W C,Jia P Y. Physical Testing and Chemical Chemical Analysis Part B:Chemical Analysis,2010,46(12):1444申书昌,宋文成,贾鹏禹.理化检验:化学分册,2010,46(12):1444
[24] Zheng C,Wang B C,Zhu L C. Chinese Journal of Analytical Chemistry,2011,39(7):1117郑超,王伯初,祝连彩.分析化学,2011,39(7):1117
[2] Li X X,Liang X K,Feng G D,et al. Modern Instruments,2007,13(1):14李欣欣,梁学凯,冯国栋,等.现代仪器,2007,13(1):14
[3] Tumbiolo S,Gal J F,Maria P C,et al. Anal Chim,2005,95(11):757
[4] Duan G. Energy and Environment,2018(2):69段钢.能源与环境,2018(2):69
[5] Wang Y F,Shi J W,Wang L,et al. Chinese Journal of Chromatography,2015,33(4):451王玉飞,施家威,王立,等.色谱,2015,33(4):451
[6] Mei M,Huang X J. Chinese Journal of Chromatography,2016,34(12):1168梅萌,黄晓佳.色谱,2016,34(12):1168
[7] Fu R N. Chinese Journal of Analysis Laboratory,2015,34(5):602傅若农.分析试验室,2015,34(5):602
[8] Yang Y C,Hui Y Q,He X B,et al. Physical Testing and Chemical Analysis Part B:Chemical Analysis,2008,44(9):904杨宇川,辉永庆,何小波,等.理化检验:化学分册,2008,44(9):904
[9] Chen M,Yuan D X,Xu P X. Journal of Analytical Science,2002,18(5):429陈猛,袁东星,许鹏翔.分析科学学报,2002,18(5):429
[10] Ligor M,Scibiorek M,Buszewski B,et al. J Microcolumn Sep,2015,11(5):377
[11] Teresa C. J Wood Chem Tech,2014,34(3):211
[12] Chen N,Zhang Y J,Zhao W L,et al. Chinese Journal of Chromatography,2018,36(1):35陈娜,张毅军,赵万里,等.色谱,2018,36(1):35
[13] Gong T,Li F. Chemical Propellants&Polymeric Materials,2014,12(4):32宫涛,李汾.化学推进剂与高分子材料,2014,12(4):32
[14] Feng J J,Qiu H D,Liu X,et al. TrAC-Trends Anal Chem,2014,44(42):44
[15] Cao D D,Lv J X,Liu J F,et al. Anal Chim Acta,2008,611(1):56
[16] Liu H,Wang D,Ji L,et al. J Chromatogr A,2010,1217(12):1898
[17] Zeng J,Zhao C,Chong F,et al. J Chromatogr A,2013,1319(6):21
[18] Zeng J,Zhao C,Chen J,et al. J Chromatogr A,2014,1365:29
[19] Li Y,Ma M G,Zhang M,et al. Chinese Journal of Analysis Laboratory,2014,33(6):621李毅,马明广,张敏,等.分析试验室,2014,33(6):621
[20] Zhou S S,Jin P X,Wang Z Y,et al. Chinese Journal of Chromatography,2018,36(2):100周珊珊,金盼霞,王子宜,等.色谱,2018,36(2):100
[21] Es-Haghi A,Hosseini S M,Khoshhesab Z M. Anal Chim Acta,2012,742(17):74
[22] Du J J,Zhang M,Zhen Q,et al. Chinese Journal of Analytical Chemistry,2017,45(11):1662杜稼健,张敏,甄琦,等.分析化学,2017,45(11):1662
[23] Shen S C,Song W C,Jia P Y. Physical Testing and Chemical Chemical Analysis Part B:Chemical Analysis,2010,46(12):1444申书昌,宋文成,贾鹏禹.理化检验:化学分册,2010,46(12):1444
[24] Zheng C,Wang B C,Zhu L C. Chinese Journal of Analytical Chemistry,2011,39(7):1117郑超,王伯初,祝连彩.分析化学,2011,39(7):1117