碳量子点/金纳米复合材料荧光增强法测定废水中苯酚
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摘要
以碳量子点(CQDs)与氯金酸作用制得碳量子点/金(CQDs/Au)纳米复合材料,并分别采用紫外可见分光光度计、荧光分光光度计和傅立叶变换红外光谱仪对CQDs/Au进行了表征。根据苯酚可使CQDs/Au在445nm处的荧光明显增强,建立了荧光增强法测定水样中苯酚含量的新方法,同时对CQDs/Au与苯酚相互作用的条件进行了优化。于pH=4.35B-R缓冲溶液存在的条件下,在最大激发/发射波长为342nm/445nm处测定体系的荧光强度,结果表明:苯酚浓度在6.0×10~(-6)～9.0×10~(-5) mol/L范围内与体系荧光强度呈线性,相关系数为0.9952,方法检出限为5.4×10-6 mol/L。将实验方法应用于测定药厂废水样中苯酚的测定,测得结果与光度法基本一致,相对标准偏差(RSD,n=5)为1.8%～2.1%,回收率为94%～101%。
The carbon quantum dots/gold nanocomposite(CQDs/Au)was prepared by reaction between carbon quantum dots(CQDs)and chloroauric acid.Then CQDs/Au was characterized using ultraviolet and visible spectrophotometer,fluorescence spectrometer and Fourier transform infrared spectrometer.Since phenol could significantly enhance the fluorescence of CQDs/Au at 445 nm,a new determination method of phenol in water sample by fluorescence enhancement method was established.Meanwhile,the interaction conditions between CQDs/Au and phenol were optimized.The fluorescence intensity of testing system was measured at maximum excitation/emission wavelength of 342 nm/445 nm in presence of B-R buffer solution at pH=4.35.The results showed that the concentration of phenol in range of 6.0×10~(-6)-9.0×10~(-5) mol/L was linear to the fluorescence intensity of system.The linear correlation coefficient was 0.995 2.The detection limit of method was 5.4×10~(-6) mol/L.The experimental method was applied to the determination of phenol in waste water from a pharmaceutical factory.The found results were basically consistent with those obtained by spectrophotometry.The relative standard deviation(RSD,n=5)was in range of 1.8%-2.1%.The recoveries were between 94%and 101%.
The carbon quantum dots/gold nanocomposite(CQDs/Au)was prepared by reaction between carbon quantum dots(CQDs)and chloroauric acid.Then CQDs/Au was characterized using ultraviolet and visible spectrophotometer,fluorescence spectrometer and Fourier transform infrared spectrometer.Since phenol could significantly enhance the fluorescence of CQDs/Au at 445 nm,a new determination method of phenol in water sample by fluorescence enhancement method was established.Meanwhile,the interaction conditions between CQDs/Au and phenol were optimized.The fluorescence intensity of testing system was measured at maximum excitation/emission wavelength of 342 nm/445 nm in presence of B-R buffer solution at pH=4.35.The results showed that the concentration of phenol in range of 6.0×10~(-6)-9.0×10~(-5) mol/L was linear to the fluorescence intensity of system.The linear correlation coefficient was 0.995 2.The detection limit of method was 5.4×10~(-6) mol/L.The experimental method was applied to the determination of phenol in waste water from a pharmaceutical factory.The found results were basically consistent with those obtained by spectrophotometry.The relative standard deviation(RSD,n=5)was in range of 1.8%-2.1%.The recoveries were between 94%and 101%.
引文
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[2]施红林,徐祎然,李银科,等.溶剂捕集-高效液相色谱法测定卷烟主流烟气中苯酚[J].理化检验:化学分册,2010,46(7):807-812.SHI Hong-lin,XU Yi-ran,LI Yin-ke,et al.Rapid HPLCdetermination of phenol in mainstream of cigarette smoke with solvent trapping[J].Physical Testing and Chemical Analysis Part B:Chemical Analysis,2010,46(7):807-812.
[3]王天娇,林勤保,宋欢,等.超高效液相色谱-串联质谱法测定食品包装纸中的酚类化合物[J].分析测试学报,2012,29(12):1153-1157.WANG Tian-jiao,LIN Qin-bao,SONG Huan,et al.Determination of phenols in food packaging paper by ultra performance liquid chromatography tandem mass spectrometry[J].Journal of Instrumental Analysis,2012,29(12):1153-1157.
[4]吴坤,周贻兵,张卫国,等.气相色谱法测定化妆品中苯酚和氢醌的可行性及误差分析[J].微量元素与健康研究,2017,34(1):59-61.WU Kun,ZHOU Yi-bing,ZHANG Wei-guo,et al.Method feasibility and error analysis for phenol and hydroquinone determination in cosmetic by gas chromatography[J].Studies of Trace Elements and Health,2017,34(1):59-61.
[5]李薇,叶芝祥.分子印迹-化学发光分析法测定水中苯酚的研究[J].环境科学,2010,31(11):2829-2834.LI Wei,YE Zhi-xiang.Molecularly imprinted techniqueflow injection-chemoluminescence system analysis detect phenol in water[J].Environmental Science,2010,31(11):2829-2834.
[6]陈雯雯,郭永明,郑问枢,等.金纳米颗粒可视化传感器在生物分子分析中的研究进展[J].分析化学,2014,42(3):307-316.CHEN Wen-wen,GUO Yong-ming,ZHENG Wen-shu,et al.Recent progress of colorimetric assays based on gold nanoparticles for biomolecules[J].Chinese Journal of Analytical Chemistry,2014,42(3):307-316.
[7]翟宏菊,戴晓威,曹爽,等.金纳米粒子的合成、性质及其应用新进展[J].吉林师范大学学报:自然科学版,2017,38(2):13-16.ZHAI Hong-ju,DAI Xiao-wei,CAO Shuang,et al.New progress of synthesis,properties and applications of gold nanoparticles[J].Journal of Jilin Normal University:Natural Science Edition,2017,38(2):13-16.
[8]孙墨杰,赵志海,陈红梅,等.碳量子点的合成研究进展与展望[J].化学通报,2016,79(8):691-698.SUN Mo-jie,ZHAO Zhi-hai,CHEN Hong-mei,et al.Research progress and prospective of synthesizing carbon quantum dots[J].Chemistry Bulletin,2016,79(8):691-698.
[9]张彦,李敏,姜晶晶,等.荧光碳点的制备及应用研究进展[J].分析科学学报,2017,33(1):135-141.ZHANG Yan,LI Min,JIANG Jing-jing,et al.Synthesis and application of the fluorescent carbon dots[J].Journal of Analytical Science,2017,33(1):135-141.
[10]林振华,唐志姣,胡玉玲,等.贵金属纳米粒子/碳量子点复合材料的制备及应用.[J].食品安全质量检测学报,2016,7(10):3866-3870.LIN Zhen-hua,TANG Zhi-jiao,HU Yu-ling,et al.Preparation and application of noble metal nanoparticles/carbon quantum dots nanocomposites[J].Journal of Food Safety and Quality,2016,7(10):3866-3870.
[11]林海琴.碳量子点/金属纳米复合材料的制备及其在电化学传感器方面的应用[D].泉州:华侨大学,2016.
[12]Peihui Luo,Chun Li,Gaoquan Shi,et al.Sythesis of gold@carbon docts composite nanoparticles for surface enhanced Raman scattering[J]Phys.Chem.Chem.Phys.,2012,14:7360-7366.
[13]王景霞,郭新秋,王戈,等.一步法制备高量子产率碳点/金复合纳米粒子[J].实验室研究与探索,2015,34(10):4-8.WANG Jing-xia,GUO Xin-qiu,WANG Ge,et al.Onestep method to synthesize high quantum yield carbon dot/Au nanocomposite[J].Research and Exploration in Laboratory,2015,34(10):4-8.
[14]魏永巨,李娜,秦身钧.磺基水杨酸的荧光光谱与荧光量子产率[J].光谱学与光谱分析,2004,24(6):647-651.WEI Yong-ju,LI Na,QIN Shen-jun.Fluorescence spectra and fluorescence quantum yield of sulfosalicylic acid[J].Spectroscopy and Spectral Analysis,2004,24(6):647-651.
[15]Zhang Jia,Dong Liang,Yu Shu-hong.A selective sensor for cyanide ion(CN-)based on the inner filter effect of metal nanoparticles with photoluminescent carbon dots as the fluorophore[J].Science Bulletin,2015,60:785-791.