多波长负吸收褪色光度法测定微量亚硝酸根及其反应机理

采用负吸收光谱校正技术,研究了在1.0 mol.dm-3盐酸介质中,亚硝酸根与吖啶黄反应的吸收光谱。基于负吸光度值或吸光度之和AT值在一定范围内与亚硝酸根浓度呈线性关系,建立了多波长负吸收褪色光度法测定痕量亚硝酸根的动力学新方法,线性范围7.2×10-6~3.6×10-4mol.dm-3,RSD 1.06%~3.12%,CV(recovery)98.00%~100.20%。方法用于环境水样中亚硝酸根的测定,准确度高,选择性好,多数常见离子无干扰,结果满意可靠。初步探讨了反应机理,根据反应体系中吸收峰的变化与溶液酸度、试剂加入顺序、溶液温度、反应时间、介质酸的种类等因素的关系,认为,在适宜的pH值、温度及有序加入介质的条件下,吖啶黄与亚硝酸根发生的是重氮化偶联反应。

Multi-Wavelength Negative Absorption Fading Spectrophotometry to Determine Trace Nitrite and It's Mechanism

Using negative absorption rectifyingtechniquie, the authors investigated spectra of the reaction of nitrite with acridine yellow in 1.0 mol x dm(-3) (1 dm = 10 cm = 0.1 m) hydrochloric medium. The authors established the new dynamics method of mensuratiog trace nitrous acid radical by the negative absorption undertint spectrophotometry at multi-wavelengths, based on the linear relation between the negative absorbance value or the AT value of absorbance sum and the nitrous acid radical concetration in a certain range. The linear range was 7.2 x 10(-6) -3.6 x 10(-4) mol x dm(-3), RSD was 1.06%-3.12%, and CV (recovery) was 98.00%-100.20%. In application to the determination of nitrite in environmental water sample, satisfactory result was abtained with high accuracy, better selectivity and common ions ceasing to effect measuring. According to the change in the absorption peak value in the reactive system,the liquor acidity, the different order for added reagent, liquor temperature, reactive time, acid kind etc., the authors believe that the reaction of acridine yellow with mitrite is diazotization-coupling, under the condition of feasible pH value, temperature, and additive order of midium.