光谱学与光谱分析 |
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Determination of Trace Amounts of Nitrite and Its Chemical Reaction Kinetics |
LUO Zhi-yong1, ZHENG Huai-li2 |
1. School of Chemistry and Chemical Engineering, Chongqing University, Chongqing 400044, China 2. Key Laboratory of the Three Georges Reservoir Region Eco-Environment of Ministry of Education, Chongqing University, Chongqing 400045, China |
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Abstract A catalytic kinetic spectrophotometric method for the determination of nitrite, NO2--S2O2-8-MR, was developed. It is based on the fading reaction of methyl red (MR) oxidized by potassium persulfate which can be catalyzed by NO-2 in the medium of dilute HCl. The optimum experimental conditions were gained by combining single factor experiments with orthogonal experiments. Calibration curve, detection limit, precision, and anti-interference under the optimum experimental conditions were researched. Its kinetics principles and parameters were discussed. Its quantitative principle was investigated. The results show that the optimum experimental conditions of this method should be as follows: 1.0 mL 0.3 mol·L-1 HCl,1.0 mL 0.01 mol·L-1 K2S2O8,0.6 mL 0.2 g·L-1 MR,reaction temperature 80 ℃ and reaction time 9 min. The principles for the quantitative determination of trace nitrite is that variation of MR concentration at the maximum absorption wavelength of 518 nm, ln(A0/A), shows a good linear relationship with the concentration of NO-2 under the optimum experimental conditions. Its determination range is 0.01~0.80 mg·L-1 and its detection limit is 0.007 mg·L-1. The kinetic characteristics are that the reaction order in NO-2 is 1 and the fading reaction is a pseudo first order reaction. Its apparent activation energy is 85.04 kJ·mol-1. Its apparent rate constant is 0.021 4 min-1, and the half-life is 32.39 min at 80 ℃. The kinetic principle is that the variation of MR concentration is directly proportional to the concentration of NO-2, ln(A0/A)=kcNO-2. This new method for the determination of trace nitrite has never previously been reported in the published literature so far. It is highly sensitive and selective. Most of the common ions don’t interfere with the determination of nitrite. This method has the advantages of convenient operation and the regents used are cheap and nontoxic. It was applied to the determination of trace nitrite in food and water samples with satisfactory results.
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Received: 2013-10-17
Accepted: 2014-02-04
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Corresponding Authors:
LUO Zhi-yong
E-mail: luozy@cqu.edu.cn
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