發(fā)布時間：2018-07-05 13:30

  本文選題：苯酚 + 亞硝酸根�。� 參考：《南華大學(xué)》2013年碩士論文

【摘要】：本文第一章分別簡述了苯酚、汞、亞硝酸根和苯乙烯的衛(wèi)生檢測的研究意義及研究現(xiàn)狀。 本文第二章建立了在醋酸介質(zhì)中，1-萘胺的熒光阻抑法測定環(huán)境中痕量苯酚的新方法。研究了體系的熒光光譜、紫外光譜特征；考察了溶液介質(zhì)、試劑用量、增敏劑的選擇、反應(yīng)時間和反應(yīng)溫度對實驗靈敏度的影響，選擇了最佳的實驗條件。實驗結(jié)果表明，在醋酸介質(zhì)中，苯酚濃度為4.36×10~(-3)μg/mL～0.35μg/mL時，體系的ΔF值與苯酚的濃度之間具有良好的線性關(guān)系，回歸方程為ΔF=36.91+309.56ρ (ρ: μg/mL)，相關(guān)系數(shù)為0.997，檢出限為1.30×10~(-3)μg/mL。用于水樣中苯酚的檢測，樣品的回收率為96.0%～104.5%。 本文第三章應(yīng)用2-(2-吡啶基)苯并咪唑熒光物與汞離子結(jié)合形成配合物2-PBI-Hg2+，使體系的熒光猝滅，其猝滅程度與汞離子的濃度有關(guān)，據(jù)此建立了汞的2-PBI熒光猝滅檢測法。實驗考察了體系的紫外光譜、熒光光譜特征。并且對影響體系的熒光強度的外部因素和催化反應(yīng)條件等進(jìn)行了優(yōu)化，確定了汞濃度與體系的ΔF的線性關(guān)系。實驗結(jié)果表明，在優(yōu)化的實驗條件下，汞離子濃度為8.27×10~(-8)~4.0×10~(-6)mol/L時，體系的ΔF值與汞離子濃度呈線性關(guān)系。線性回歸方程為ΔF=125.44c+16.75(c為硝酸汞的濃度，×10~(-6)mol/L)，相關(guān)系數(shù)r=0.997。方法的檢測限為2.41×10~(-8)mol/L。該方法精密度好、操作簡便、靈敏度高，應(yīng)用于環(huán)境中痕量汞的測定結(jié)果較好。 本文第四章研究了環(huán)境中痕量的亞硝酸鹽的反相-高效液相色譜測定方法。該方法根據(jù)亞硝酸根離子氧化吖啶紅，使吖啶紅(AR)的熒光強度猝滅，用HPLC熒光檢測器檢測AR的色譜峰面積,據(jù)此建立了ΔU與ρNO2-的定量關(guān)系。實驗優(yōu)化了色譜條件，色譜柱：Agilent TC-C18(4.6mm×150mm,5μm；美國安捷倫公司)；流動相：甲醇-乙腈-0.1%三氯乙酸(50∶25∶25v/v)，流速為1.0mL/min；熒光檢測波長：λ_(ex)=530nm，λ_(em)550nm；柱溫：30℃；進(jìn)樣量：20μL。亞硝酸根離子濃度為10.0～400.0ng/mL時，ΔU與亞硝酸根離子濃度之間呈現(xiàn)線性定量關(guān)系，ΔU=108.72ρ+70.58，相關(guān)系數(shù)為r=0.998。檢出限為1.50ng/mL，用于環(huán)境水樣中痕量亞硝酸鹽測定，加標(biāo)回收率為93.3%～106.8%。 本文第五章建立了一次性飯盒中殘余苯乙烯的反相高效液相色譜檢測方法，分析了它在5種提取液中的溶出特性。實驗優(yōu)化選擇色譜條件為： TC-C18色譜柱，，流動相為甲醇和水的比例為90∶10，流速為1.0mL/min，進(jìn)樣量為20μL，柱溫為45℃，測定波長為245nm。實驗結(jié)果表明，在苯乙烯質(zhì)量濃度為0.05～90.00μg/mL時，A=2.45ρ－0.18，r=0.9997，檢出限為0.03μg/mL，回收率為92.00%～107.00%，該方法靈敏度高，重現(xiàn)性好。檢測一次性飯盒中的殘余苯乙烯，結(jié)果滿意。
[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

本文編號：2100359