腐植酸/凹土复合材料分离富集-火焰原子吸收光谱法测定蔬菜中痕量铅(Ⅱ)
FAAS Determination of Trace Amount of Pb(Ⅱ) in Vegetables After Separation and Preconcentration with Humic Acid/Attapulgite Compound Material
摘 要
蔬菜试样用硝酸-过氧化氢(7+4)溶液溶解后,以腐植酸/凹土复合材料(HACM)分离富集样品溶液中的痕量铅(Ⅱ),1.5 mol·L-1硝酸-甲基异丁酮溶液进行淋洗分离,流量为10.0 mL·min-1,采用火焰原子吸收光谱法测定蔬菜中痕量铅(Ⅱ)。在优化的试验条件下,HACM对铅(Ⅱ)的动态吸附容量为40.98 mg·g-1。铅(Ⅱ)的质量浓度在0.32~5.12 mg·L-1范围内与吸光度呈线性关系,方法的检出限(3σ)为0.32 μg·L-1。方法用于分析蔬菜样品,并用标准加入法做回收试验,测得回收率在96.2%~104.4%之间,测定值的相对标准偏差(n=6)均小于2%。
腐植酸/凹土复合材料
铅(Ⅱ)
蔬菜
FAAS
Humic acid/attapulgite compound materials
Pb(Ⅱ)
Vegetable
Abstract
The vegetable sample was dissolved in a mixed solution of HNO3 and H2O2 (7+4). Trace amount of Pb(Ⅱ) in the sample solution was separated and preconcentrated on humic acid/attapulgite compound material (HACM), and eluted from FACM with 1.5 mol·L-1 nitric acid-methyl isobutyl ketone at the flow-rate of 10.0 mL·min-1. The dynamic adsorption capacity of Pb(Ⅱ) on HACM obtained was 40.98 mg·g-1. Linear relationship between values of absorbance and mass concentration of Pb(Ⅱ) was obtained in the range of 0.32-5.12 mg·L-1, with detection limit (3σ) of 0.32 μg·L-1. The proposed method was used in the analysis of vegetable samples, and recovery was tested by standard addition method giving values of recovery in the range of 96.2%-104.4% with RSD′s (n=6) less than 2%.
中图分类号 O657.31
所属栏目 工作简报
基金项目 淮安市工业支撑项目(HAG2010013)
收稿日期 2011/7/15
修改稿日期
网络出版日期
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备注蒋顶云(1966-),女,江苏淮安人,高级工程师,主要研究方向为化学合成与分析。
引用该论文: JIANG Ding-yun,SHI Ying-ying,XIONG Qing-ping,TANG Ru-miao. FAAS Determination of Trace Amount of Pb(Ⅱ) in Vegetables After Separation and Preconcentration with Humic Acid/Attapulgite Compound Material[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2012, 48(9): 1051～1054
蒋顶云,石莹莹,熊清平,唐如苗. 腐植酸/凹土复合材料分离富集-火焰原子吸收光谱法测定蔬菜中痕量铅(Ⅱ)[J]. 理化检验－化学分册, 2012, 48(9): 1051～1054
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【3】MESTOR Z, PAWLISZYN J. Speciation of dimethylarsinic acid and monomethylarsonic acid by SPME gas chromatography ion trap mass spectrometry［J］. Chromatography, 2000,873(1):129-135.
【4】刘正华,周方钦,黄荣辉,等.纳米二氧化钛对痕量铅的吸附性能研究［J］.分析试验室, 2006,25(11):63-66.
【5】CHAO Lu, GUANG Qun-song, JIN Ming-lin, et al. Enhancement in sample preconcentration by the on-line incorporation of cloud point extraction to flow injection analysis inside the chemiluminescence cell and the determination of total serum bilirubin［J］. Anal Chim Acta, 2007,590(2):159-165.
【6】艾军,李德龙,汤志勇.流动注射在线液-液萃取火焰原子吸收法测定水中痕量铅［J］.分析科学学报, 2001,17(5):414-417.
【7】任红英,周方钦,李改云,等.纳米硅羟基磷灰石分离富集-火焰原子吸收法测定水样中痕量铅［J］.分析科学学报, 2010,26(1):63-66.
【8】高甲友.流动注射-在线富集火焰原子吸收分光光度法测定痕量铅［J］.分析科学学报, 2007,23(4):489-491.
【9】苏耀东,黄燕,赫冰冰,等.吡咯烷二硫代氨基甲酸铵-Ni(Ⅱ)快速共沉淀分离富集和原子吸收光谱法测定痕量铜、铅和镉［J］.分析科学学报, 2007,23(2):173-176.
【10】蒋桂华,刘春明,王晓菊.准液膜分离富集-火焰原子吸收法测定痕量镁、铅［J］.光谱学与光谱分析, 1999,19(5):732-733.
【11】孙梅,吴强华.浊点萃取富集-石墨炉原子吸收光谱法同时测定环境水样和中药中超痕量铅和镉［J］.理化检验-化学分册, 2009,45(6):710-713.
【12】张强华,石莹莹,熊清平,等.分子印迹壳聚糖/凹土分离富集火焰原子吸收光谱测定痕量铅［J］.应用化学, 2011,28(9):1073-1081.
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