苯酚、汞、亚硝酸根和苯乙烯检测新方法研究

发布时间：2018-07-05 13:30

  本文选题：苯酚 + 亚硝酸根　； 参考：《南华大学》2013年硕士论文

【摘要】：本文第一章分别简述了苯酚、汞、亚硝酸根和苯乙烯的卫生检测的研究意义及研究现状。 本文第二章建立了在醋酸介质中，1-萘胺的荧光阻抑法测定环境中痕量苯酚的新方法。研究了体系的荧光光谱、紫外光谱特征；考察了溶液介质、试剂用量、增敏剂的选择、反应时间和反应温度对实验灵敏度的影响，选择了最佳的实验条件。实验结果表明，在醋酸介质中，苯酚浓度为4.36×10~(-3)μg/mL～0.35μg/mL时，体系的ΔF值与苯酚的浓度之间具有良好的线性关系，回归方程为ΔF=36.91+309.56ρ (ρ: μg/mL)，相关系数为0.997，检出限为1.30×10~(-3)μg/mL。用于水样中苯酚的检测，样品的回收率为96.0%～104.5%。 本文第三章应用2-(2-吡啶基)苯并咪唑荧光物与汞离子结合形成配合物2-PBI-Hg2+，使体系的荧光猝灭，其猝灭程度与汞离子的浓度有关，据此建立了汞的2-PBI荧光猝灭检测法。实验考察了体系的紫外光谱、荧光光谱特征。并且对影响体系的荧光强度的外部因素和催化反应条件等进行了优化，确定了汞浓度与体系的ΔF的线性关系。实验结果表明，在优化的实验条件下，汞离子浓度为8.27×10~(-8)~4.0×10~(-6)mol/L时，体系的ΔF值与汞离子浓度呈线性关系。线性回归方程为ΔF=125.44c+16.75(c为硝酸汞的浓度，×10~(-6)mol/L)，相关系数r=0.997。方法的检测限为2.41×10~(-8)mol/L。该方法精密度好、操作简便、灵敏度高，应用于环境中痕量汞的测定结果较好。 本文第四章研究了环境中痕量的亚硝酸盐的反相-高效液相色谱测定方法。该方法根据亚硝酸根离子氧化吖啶红，使吖啶红(AR)的荧光强度猝灭，用HPLC荧光检测器检测AR的色谱峰面积,据此建立了ΔU与ρNO2-的定量关系。实验优化了色谱条件，色谱柱：Agilent TC-C18(4.6mm×150mm,5μm；美国安捷伦公司)；流动相：甲醇-乙腈-0.1%三氯乙酸(50∶25∶25v/v)，流速为1.0mL/min；荧光检测波长：λ_(ex)=530nm，λ_(em)550nm；柱温：30℃；进样量：20μL。亚硝酸根离子浓度为10.0～400.0ng/mL时，ΔU与亚硝酸根离子浓度之间呈现线性定量关系，ΔU=108.72ρ+70.58，相关系数为r=0.998。检出限为1.50ng/mL，用于环境水样中痕量亚硝酸盐测定，加标回收率为93.3%～106.8%。 本文第五章建立了一次性饭盒中残余苯乙烯的反相高效液相色谱检测方法，分析了它在5种提取液中的溶出特性。实验优化选择色谱条件为： TC-C18色谱柱，，流动相为甲醇和水的比例为90∶10，流速为1.0mL/min，进样量为20μL，柱温为45℃，测定波长为245nm。实验结果表明，在苯乙烯质量浓度为0.05～90.00μg/mL时，A=2.45ρ－0.18，r=0.9997，检出限为0.03μg/mL，回收率为92.00%～107.00%，该方法灵敏度高，重现性好。检测一次性饭盒中的残余苯乙烯，结果满意。
[Abstract]:In the first chapter, the significance and present situation of hygienic detection of phenol, mercury, nitrite and styrene were reviewed. In chapter 2, a new method for the determination of trace phenol in acetic acid medium by fluorescence inhibition method is established. The effects of solution medium, reagent dosage, sensitizer selection, reaction time and reaction temperature on the experimental sensitivity were studied, and the optimum experimental conditions were selected. The experimental results show that there is a good linear relationship between 螖 F value and phenol concentration when phenol concentration is 4.36 脳 10 ~ (-3) 渭 g / m ~ (-1) 渭 g / mL in acetic acid medium. The regression equation is 螖 F ~ (36.91) 蟻 (蟻: 渭 g / mL), the correlation coefficient is 0.997, and the detection limit is 1.30 脳 10 ~ (-3) 渭 g / mL. The method has been applied to the determination of phenol in water. The recovery rate of the sample is 96. 0% 104.5%. In the third chapter, the complex 2-PBI-Hg2 was formed by the combination of 2- (2-pyridyl) benzimidazole fluorescence with mercury ion, and the quenching degree was related to the concentration of mercury ion. Based on this, a fluorescence quenching method for 2-PBI was established. The UV and fluorescence spectra of the system were investigated experimentally. The external factors affecting the fluorescence intensity of the system and the catalytic reaction conditions were optimized, and the linear relationship between mercury concentration and 螖 F of the system was determined. The experimental results show that under the optimized experimental conditions, the 螖 F value of the system is linear to the mercury ion concentration when the mercury ion concentration is 8.27 脳 10 ~ (-8) or 4.0 脳 10 ~ (-6) mol / L. The linear regression equation is 螖 F _ (125.44) c 16.75 (c is the concentration of mercury nitrate, 脳 10 ~ (-6) mol / L), and the correlation coefficient is 0.997. The detection limit of the method is 2.41 脳 10 ~ (-8) mol / L. The method has the advantages of good precision, simple operation and high sensitivity. It has been applied to the determination of trace mercury in the environment. In chapter 4, a method for the determination of trace nitrite in the environment by reversed-phase-high-performance liquid chromatography (HPLC) has been studied. According to the oxidation of acridine red by nitrite ion, the fluorescence intensity of acridine red (AR) was quenched. The peak area of AR was detected by HPLC fluorescence detector, and the quantitative relationship between 螖 U and 蟻 NO2- was established. The chromatographic conditions were optimized as follows: column 1: Agilent TC-C18 (4.6mm 脳 150mm); mobile phase: methanol-acetonitrile-0.1% trichloroacetic acid (50:25:25v/v), flow rate 1.0 mL / min; fluorescence detection wavelength: 位 _ (ex) 530nm, 位 _ (em) _ 550nm; column temperature: 30 鈩

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