基于鲁米诺-H2O2混合溶液作为发光液与海水中NO发生反应产生发光信号的原理,提出了一种测定海水中痕量NO的化学发光法。确定了化学发光法测定NO的最佳条件:pH9.2、浓度1×10-2 mol/dm3的碳酸盐为缓冲体系,鲁米诺浓度为8.4×10-5 mol/dm3,H2O2浓度为1×10-2 mol/dm3,测定温度为20℃。该方法在最佳实验条件下,当NO浓度在1.4×10-12~9.8×10-10 mol/dm3范围内,其浓度值与发光峰面积呈良好的线性关系,相关系数R=0.997,P〈0.000 1。该方法的检出限为1.4×10-12 mol/dm3(S/N=3),相对标准偏差(RSD)为13.6%(1.2×10-11 mol/dm3)。采用该方法对胶州湾表层海水中NO的分布进行了初步研究,结果表明,NO浓度范围为未检出~7.1×10-11 mol/dm3,平均浓度为(1.6±1.8)×10-11 mol/dm3。
A chemiluminescence method measuring the concentration of NO in seawater was established in this paper on the base of a reaction between the mixed solution of luminol-H2O2,the chemiluminescence probe,and NO,in which the chemiluminescence signal was emitted.The optimal results in the determination of NO concentration were under the conditions of a pH 9.2 buffer system with 1×10-2 mol/dm3 carbonate,8.4×10-5 mol/dm3 luminol,1×10-2 mol/dm3 H2O2,and under 20 ℃ and 1×10-3 mol/dm3 EDTA as a optimal masking agent.Under these optimal conditions,there was a significant linear relationship between the NO concentration and the peak area of chemiluminescence signal in the range of NO concentration from 1.4×10-12 to 9.8×10-10 mol/ dm3(R=0.997,P 0.000 1).The detection limit for NO was 1.4×10-12 mol/dm3(S/N).In 7 times of parallel determination to 1.2×10-11 mol/dm3NO aqueous solution,the relative standard deviation(RSD) was 13.6%.The NO concentration in the surface seawater of Jiaozhou Bay,China was successfully determined using this method and the results indicated that the concentrations of NO ranged from undetected to 7.1×10-11 mol/ dm3 with an average of(1.6±1.8)×10-11 mol/dm3.