Gonzáles A P S, Firmino M A, Nomura C S, Rocha F R P, Oliveira P V, Gaubeur I
Centro de Ciências Naturais e Humanas, Universidade Federal do ABC, Rua Santa Adélia, 166, 09210-170 Santo André, Brazil.
Anal Chim Acta. 2009 Mar 23;636(2):198-204. doi: 10.1016/j.aca.2009.01.047. Epub 2009 Feb 1.
The physical and chemical characteristics of peat were assessed through measurement of pH, percentage of organic matter, cationic exchange capacity (CEC), elemental analysis, infrared spectroscopy and quantitative analysis of metals by ICP OES. Despite the material showed to be very acid in view of the percentage of organic matter, its CEC was significant, showing potential for retention of metal ions. This characteristic was exploited by coupling a peat mini-column to a flow system based on the multicommutation approach for the in-line copper concentration prior to flame atomic absorption spectrometric determination. Cu(II) ions were adsorbed at pH 4.5 and eluted with 0.50 molL(-1) HNO(3). The influence of chemical and hydrodynamic parameters, such as sample pH, buffer concentration, eluent type and concentration, sample flow-rate and preconcentration time were investigated. Under the optimized conditions, a linear response was observed between 16 and 100 microgL(-1), with a detection limit estimated as 3 microgL(-1) at the 99.7% confidence level and an enrichment factor of 16. The relative standard deviation was estimated as 3.3% (n=20). The mini-column was used for at least 100 sampling cycles without significant variation in the analytical response. Recoveries from copper spiked to lake water or groundwater as well as concentrates used in hemodialysis were in the 97.3-111% range. The results obtained for copper determination in these samples agreed with those achieved by graphite furnace atomic absorption spectrometry (GFAAS) at the 95% confidence level.
通过测量pH值、有机质百分比、阳离子交换容量(CEC)、元素分析、红外光谱以及采用电感耦合等离子体发射光谱法(ICP OES)对金属进行定量分析,评估了泥炭的物理和化学特性。尽管从有机质百分比来看该材料呈强酸性,但其阳离子交换容量显著,显示出保留金属离子的潜力。基于多通道进样方法,将泥炭微型柱与流动系统联用,用于在火焰原子吸收光谱测定之前对铜进行在线富集,利用了这一特性。Cu(II)离子在pH 4.5时被吸附,并用0.50 molL(-1) HNO(3)洗脱。研究了化学和流体动力学参数的影响,如样品pH值、缓冲液浓度、洗脱液类型和浓度、样品流速和富集时间。在优化条件下,在16至100 microgL(-1)之间观察到线性响应,在99.7%置信水平下估计检测限为3 microgL(-1),富集因子为16。相对标准偏差估计为3.3%(n = 20)。该微型柱至少用于100个采样循环,分析响应无显著变化。加标到湖水或地下水中的铜以及血液透析中使用的浓缩物的回收率在97.3 - 111%范围内。在95%置信水平下,这些样品中铜测定的结果与石墨炉原子吸收光谱法(GFAAS)获得的结果一致。