Abstract:The potassium periodate could oxidize the hydrazine yellow in sulfuric acid medium, leading to the decrease of absorbance. The addition of iron (III) could obviously catalyze this reaction. Moreover, the catalytic extent was related to the concentration of added iron (III). Based on this, the determination method of trace iron (III) by hydrazine yellow fading catalytic kinetic spectrophotometry was established. The effect of different testing conditions on sensitivity of catalytic reaction was investigated. The optimal experimental conditions were obtained: 4.0 mL of sulfuric acid; 0.9 mL of potassium periodate solution; 1.5 mL of hydrazine yellow solution; the reaction temperature of 100 ℃; the reaction time of 9 min. In addition, the influence of several common metal and nonmetal ions on the reaction was investigated, including Na+, K+, Cl- and SO42-. It was found that most common ions had no or little interference with the determination. Under the optimal determination conditions, the maximum absorption peak of system was 427 nm, the catalytic reaction rate constant was 9.8×10-4/s, and the apparent activation energy was 23.63 kJ/mol. The calibration curve was linear when the mass concentration of iron was in range of 2.4-40 μg/L, and the correlation coefficient was r=0.998 7. The detection limit of method was 2.4×10-7 g/L. The proposed method was applied to the determination of iron in natural water. The relative standard deviations (RSD, n=6) were between 1.7% and 2.4%. The found results were consistent with those obtained by flame atomic absorption method.
刘斌, 常薇, 杜燕萍, 郁翠华, 李维. 高碘酸钾氧化肼黄褪色催化动力学光度法测定铁[J]. 冶金分析, 2016, 36(8): 52-55.
LIU Bin, CHANG Wei, DU Yan-ping, YU Cui-hua, LI Wei. Determination of iron by catalytic kinetic spectrophotometry based on the oxidization fading reaction of hydrazine yellow with potassium periodate. , 2016, 36(8): 52-55.
白石花,莫平英,陈吉祥.电感耦合等离子体原子发射光谱法测定锌铝合金中锡铅铁[J].冶金分析,2014,34(11):77-80.BAI Shi-hua,MO Ping-ying,CHEN Ji-xiang.Determination of tin,lead and iron in zinc-aluminum alloy by inductively coupled plasma atomic emission spectrometry[J].Metallurgical Analysis,2014,34(11):11-80.
[2]
Cubadda F,Raggi A.Determination of cadmium,lead,iron,nickel and chromium in selected food matrices by plasma spectrometric techniques[J].Microchemical Journal,2005,79 (s1-2):91- 96.
[3]
Gómez-Nieto B,Gismera M J,Sevilla M T,et al.Simultaneous and direct determination of iron and nickel in biological solid samples by high-resolution continuum source graphite furnace atomic absorption spectrometry[J].Talanta,2013,116(22):860-865.
[4]
王中瑗,张宏康,方宏达,等.流动注射编结反应器火焰原子吸收光谱法测定水样中三价铁和二价铁[J].冶金分析,2012,32(4):57-61.WANG Zhong-yuan,ZHANG Hong-kang,FANG Hong-da,et al.Flow injection-knotted reactor coupled with flame atomic absorption spectrometry for the determination of iron and iron(II) in water samples[J].Metallurgical Analysis,2012,2(4):57-61.
[5]
Peng B,Shen Y L,Gao Z T,et al.Determination of total iron in water and foods by dispersive liquid-liquid microextraction coupled with microvolume UV-vis spectrophotometry[J].Food Chemistry,2015,176:288-293.
[6]
谢建鹰,陈宗保,雷明建.铁(Ⅲ)-酚藏花红-溴酸钾体系催化动力学光度法测定铁[J].冶金分析,2011,31(8):36-39.XIE Jian-ying,CHEN Zong-bao,LEI Ming-jian.Catalytic kinetic spectrophotome tric determination of iron in iron-phenosafranine-potassium bromate system[J].Metallurgical Analysis,2011,31(8):36-39.
[7]
侯法菊,陈玉静,苗延虹,等.双波长双指示剂催化动力学光度法测定痕量Fe(Ⅲ) [J].分析科学学报,2015,31(2):294-296.HOU Fa-ju,CHEN Yu-jing,MIAO Yan-hong,et al.Dual-wavelength dual-indicator catalytic kinetic spectrophotometry for determination of trace Fe[J].Journal of Analytical Science,2015,31(2):294-296.
[8]
Ghoneim E M.Simultaneous determination of Mn(II),Cu(II) and Fe as 2-(5′-bromo-2′-pyridylazo)-5-diethylaminophenol complexes by adsorptive cathodic stripping voltammetry at a carbon paste electrode[J].Talanta,2010,82:646-652.
[9]
李艳霞,贾华丽,李玖零.阻抑溴酸钾氧化乙基橙褪色动力学极谱法测定痕量铁[J].冶金分析,2012,32(1):56-59.LI Yan-xia,JIA Hua-li,LI Jiu-ling.Determination of trace iron by kinetic polarography based on inhibitory fading of ethyl orange oxidized by potassium bromate[J].Metallurgical Analysis,2012,32(1):56-59.
[10]
翟好英,邹豪,陈瑜,等.羧甲基壳聚糖共振散射法测定铁(Ⅲ) [J].冶金分析,2015,35(9):58-61.ZHAI Hao-ying,ZOU Hao,CHEN Yu,et al.Determination of iron by resonance scattering method with carboxymethyl chitosan[J].Metallurgical Analysis,2015,35(9):58-61.
[11]
赵怀颖,温宏利,夏月莲,等.无汞重铬酸钾-自动电位滴定法准确测定矿石中的全铁含量[J].岩矿测试,2012,31(3):473-478.ZHAO Huai-ying,WEN Hong-li,XIA Yue-lian,et al.Accurate determination of total iron in ores by automatic potentiometric titration without potassium dichromate[J].Rock and Mineral Analysis,2012,31(3):473-478.