流动注射法监测食品用水中重金属突发性污染
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摘要
食品用水突发性污染事件的发生呈上升趋势,食品用水安全面临挑战,加强对食品用水突发性污染的在线监测已成为各级政府突发事件应急管理的研究重点。
本文以铅、镉、汞离子为对象,研究食品用水中重金属突发性污染的早期快速预警。主要内容包括(1)食品用水电导率、pH值变化和化学污染物的关系；(2)流动注射发光细菌(青海弧菌Q67)监测食品用水突发性重金属污染的适用性；(3)流动注射二甲酚橙分光光度法检测食品用水中铅离子；(4)流动注射P矩阵分光光度法测定食品用水中镉离子。主要结果如下：
1.金属离子浓度的增加可引起电导率的增大,但在标准值的1000倍以下增加的幅度很小,与空白对照差异不显著,只有当金属离子超过饮用水标准的1万倍时,才会引起电导和pH值的显著变化。且Pb2+浓度与电导率的相关性小。
2.建立了流动注射系统与生物发光检测仪相结合的体系,采用新鲜培养的发光细菌(pH 6.75培养17 h的青海弧菌Q67菌悬液)为实验菌测定重金属。拟合发光抑制率-浓度曲线,进而推断出三种重金属Hg2+、Pb2+、Cd2+的EC50分别为0.57 mg/L、20.58 mg/L、10.51mg／L,毒性大小为Hg2+>Cd2+>Pb2+。
3.通过580 nm处测定XO与Pb(Ⅱ)生成的紫红色螯合物的吸光值,建立流动注射二甲酚橙分光光度法测定Pb(Ⅱ)的方法。该方法以1.5×10-3mol/L的XO为显色剂,1%的Triton X-100为增敏剂,0.02 mol/L(pH=5)的醋酸-醋酸钠作缓冲液,。测定Pb(Ⅱ)在2～10 mg／L范围内成线性,最低检出限为0.164 mg／L。
4.在pH9.0的NH4Cl-NH3·H2O缓冲体系下,镉、锌、铜与显色剂2-(5-溴-2-吡啶偶氮)-5-二乙氨基酚(5-Br-PADAP)发生显色反应。在400～700 nm波长下,建立P矩阵多元回归校正模型,Cu2+的回收率接近100%,Cd2+回收率在另两种离子浓度很小时,回收率分别为95.8和104.0%,但当Cu2+、Zn2+浓度很大,而Cd2+浓度很小时,回收率仅为78.9%。
结果表明,流动注射分光光度法和化学计量技术的联用,有可能实现对食品用水重金属突发性污染的在线监测和预警。
Emergency pollution of food water incidence is increasing and the safety of drink water face serious challege. Unknown sudden pollution of food water is one of the key research areas in the emergency management adminishered by governments. The purpose of this study was to investigate the possibility of the early warning of heavy metal such as lead, cadmium and mecury sudden pollution in food water, with the main content:
(1) Evaluation of the correlation between the electric conductivity, pH value and heavy metal pollution; (2) Determination of Hg(Ⅱ), Pb(Ⅱ) and Cd(Ⅱ) with V. qinhaiensis by coupling flow injection-bioluminescence method; (3) Determination of Pb(Ⅱ) by flow injection analysis(FIA) spectrophotometry. (4) Determination of Cd(Ⅱ) in drinking water by FIA spectrophotometry using chemometrics-p matrix. The main results were as follows:
(1) There were positive correlation between electric conductivity and the concentration of heavy metals, but the discrepancy wasn't significant when the concentration was below in 1000 times of the maximum levels for GB prescribled, except for Pb(Ⅱ).
(2) An on-line FIA combined with luminescent instrument was set up to detect the metal ions via freshly prepared luminescent bacteria suspension (Vibro qinhaiensis sp.Q67 suspension were at the optimum cultivation pH of 6.75 for 17 h). Fit the luminescent inhibition-metal concentration line, it was indicated that 50% effective concentration (EC50) of Hg(Ⅱ), Pb(Ⅱ) and Cd(Ⅱ) were 0.57 mg/L,20.58 mg/L and 10.51 mg/L respectively. And the toxicity sequence from large to small was:Hg2+, Cd2+, Pb2+.
(3) Based on the maximum absorption of the Pb(II)-xylenol orange (XO) complex was at 580 nm, determination of lead by using FIA with spectrophotometric was constructed. The results were showed that a solution 1.5×10-3mol/L XO in 0.02 mol/L acetate buffer (pH 5.0), in the presence of triton X-100 led to the sensitive color reaction of lead and XO, and it followed the beer's law in the concentration range of 2-10 mg/L with the LOD of 0.164 mg/L.
(4) At the buffer solution (pH 9.0) of NH4Cl-NH3.H2O, the Zn2+, Cu2+, Cd2+were colored with 2-[(Bromo-2-pyridyl)-azo]-5-diethyl-aminophenol. Under the absorbent spectrum of 400-700 nm wavelength, the concentration of Cd(Ⅱ) was predicted with P-matrix model. The recoveries of Cu2+was approximately to 100%, and the Cd2+was 95.8-104.0% when Cu2+and Zn2+ were in low concentration.
Rusults above concludes that combination of FIA, spectrophotometry and P-matrix model could detect the emergency pollution of heavy metals in the food water and alarm early this pollution on-line.
本文以铅、镉、汞离子为对象,研究食品用水中重金属突发性污染的早期快速预警。主要内容包括(1)食品用水电导率、pH值变化和化学污染物的关系；(2)流动注射发光细菌(青海弧菌Q67)监测食品用水突发性重金属污染的适用性；(3)流动注射二甲酚橙分光光度法检测食品用水中铅离子；(4)流动注射P矩阵分光光度法测定食品用水中镉离子。主要结果如下：
1.金属离子浓度的增加可引起电导率的增大,但在标准值的1000倍以下增加的幅度很小,与空白对照差异不显著,只有当金属离子超过饮用水标准的1万倍时,才会引起电导和pH值的显著变化。且Pb2+浓度与电导率的相关性小。
2.建立了流动注射系统与生物发光检测仪相结合的体系,采用新鲜培养的发光细菌(pH 6.75培养17 h的青海弧菌Q67菌悬液)为实验菌测定重金属。拟合发光抑制率-浓度曲线,进而推断出三种重金属Hg2+、Pb2+、Cd2+的EC50分别为0.57 mg/L、20.58 mg/L、10.51mg／L,毒性大小为Hg2+>Cd2+>Pb2+。
3.通过580 nm处测定XO与Pb(Ⅱ)生成的紫红色螯合物的吸光值,建立流动注射二甲酚橙分光光度法测定Pb(Ⅱ)的方法。该方法以1.5×10-3mol/L的XO为显色剂,1%的Triton X-100为增敏剂,0.02 mol/L(pH=5)的醋酸-醋酸钠作缓冲液,。测定Pb(Ⅱ)在2～10 mg／L范围内成线性,最低检出限为0.164 mg／L。
4.在pH9.0的NH4Cl-NH3·H2O缓冲体系下,镉、锌、铜与显色剂2-(5-溴-2-吡啶偶氮)-5-二乙氨基酚(5-Br-PADAP)发生显色反应。在400～700 nm波长下,建立P矩阵多元回归校正模型,Cu2+的回收率接近100%,Cd2+回收率在另两种离子浓度很小时,回收率分别为95.8和104.0%,但当Cu2+、Zn2+浓度很大,而Cd2+浓度很小时,回收率仅为78.9%。
结果表明,流动注射分光光度法和化学计量技术的联用,有可能实现对食品用水重金属突发性污染的在线监测和预警。
Emergency pollution of food water incidence is increasing and the safety of drink water face serious challege. Unknown sudden pollution of food water is one of the key research areas in the emergency management adminishered by governments. The purpose of this study was to investigate the possibility of the early warning of heavy metal such as lead, cadmium and mecury sudden pollution in food water, with the main content:
(1) Evaluation of the correlation between the electric conductivity, pH value and heavy metal pollution; (2) Determination of Hg(Ⅱ), Pb(Ⅱ) and Cd(Ⅱ) with V. qinhaiensis by coupling flow injection-bioluminescence method; (3) Determination of Pb(Ⅱ) by flow injection analysis(FIA) spectrophotometry. (4) Determination of Cd(Ⅱ) in drinking water by FIA spectrophotometry using chemometrics-p matrix. The main results were as follows:
(1) There were positive correlation between electric conductivity and the concentration of heavy metals, but the discrepancy wasn't significant when the concentration was below in 1000 times of the maximum levels for GB prescribled, except for Pb(Ⅱ).
(2) An on-line FIA combined with luminescent instrument was set up to detect the metal ions via freshly prepared luminescent bacteria suspension (Vibro qinhaiensis sp.Q67 suspension were at the optimum cultivation pH of 6.75 for 17 h). Fit the luminescent inhibition-metal concentration line, it was indicated that 50% effective concentration (EC50) of Hg(Ⅱ), Pb(Ⅱ) and Cd(Ⅱ) were 0.57 mg/L,20.58 mg/L and 10.51 mg/L respectively. And the toxicity sequence from large to small was:Hg2+, Cd2+, Pb2+.
(3) Based on the maximum absorption of the Pb(II)-xylenol orange (XO) complex was at 580 nm, determination of lead by using FIA with spectrophotometric was constructed. The results were showed that a solution 1.5×10-3mol/L XO in 0.02 mol/L acetate buffer (pH 5.0), in the presence of triton X-100 led to the sensitive color reaction of lead and XO, and it followed the beer's law in the concentration range of 2-10 mg/L with the LOD of 0.164 mg/L.
(4) At the buffer solution (pH 9.0) of NH4Cl-NH3.H2O, the Zn2+, Cu2+, Cd2+were colored with 2-[(Bromo-2-pyridyl)-azo]-5-diethyl-aminophenol. Under the absorbent spectrum of 400-700 nm wavelength, the concentration of Cd(Ⅱ) was predicted with P-matrix model. The recoveries of Cu2+was approximately to 100%, and the Cd2+was 95.8-104.0% when Cu2+and Zn2+ were in low concentration.
Rusults above concludes that combination of FIA, spectrophotometry and P-matrix model could detect the emergency pollution of heavy metals in the food water and alarm early this pollution on-line.
引文
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