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Sorbent separation and enrichment method for cobalt ions determination by graphite furnace atomic absorption spectrometry in water and urine samples using multiwall carbon nanotubes

机译:石墨炉原子吸收光谱法测定多壁碳纳米管在水和尿液中的吸附剂分离富集方法测定钴离子

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A new cobalt ions pre-concentration method, optimised by fractional factorial design, using multiwall carbon nanotubes (MWCNTs) with further Graphite Furnace Atomic Absorption Spectrometry (GFAAS) quantification is described. The method explores the high chemical and physical stability of MWCNTs for improving the detectability of GFAAS. It is based on off-line pre-concentration of 20.0mL of sample previously buffered (pH 8.82) on MWCNTs at a flow rate of l0.0 mLmin~(-1). After the pre-concentration procedure, the elution step was carried out with 500 μL of 0.524 mol L~(-1) HNO_3 solution at a flow rate of 2.0 mLmin~(-1). Fractional factorial designs and response surface methodology were employed for optimisation of all chemical parameters involved in the pre-concentration procedure, including pre-concentration flow rate, buffer and eluent concentration, sample pH and elution volume. The method provides a linear calibration range from 0.03 up to 7.00 μg L~(-1) with linear correlation coefficient higher than 0.9994 and limits of detection and quantification of 0.01 and 0.03 μg L~(-1) respectively. Repeatability of the six measurements was found to be 2.38 and 1.84% for 0.3 and 4.5 μg L~(-1) cobalt concentration, respectively. By pre-concentrating 20.0mL of sample, a pre-concentration factor (PF) of 19.10-fold and a consumption index of 1.05 m L were obtained. The pre-concentration efficiency (PE) was found to be 9.55min~(-1). The proposed method was successfully applied for the pre-concentration and determination of cobalt in water and urine samples with satisfactory recovery values.
机译:描述了一种通过分数阶乘设计优化的新的钴离子预浓缩方法,该方法使用多壁碳纳米管(MWCNT)和进一步的石墨炉原子吸收光谱(GFAAS)定量。该方法探索了MWCNT的高化学和物理稳定性,以改善GFAAS的可检测性。它基于离线预浓缩的20.0mL样品(流速为10.0 mLmin〜(-1))预先在MWCNTs上缓冲(pH 8.82)。在预浓缩程序后,用500μL的0.524 mol L〜(-1)HNO_3溶液以2.0 mLmin〜(-1)的流速进行洗脱。分数阶乘设计和响应面方法被用于优化预浓缩过程中涉及的所有化学参数,包括预浓缩流速,缓冲液和洗脱液浓度,样品pH和洗脱体积。该方法提供的线性校正范围为0.03至7.00μgL〜(-1),线性相关系数高于0.9994,检出限和定量限分别为0.01和0.03μgL〜(-1)。发现六次测量的重复性分别为0.3和4.5μgL〜(-1)钴浓度为2.38%和1.84%。通过对20.0mL样品进行预浓缩,可获得19.10倍的预浓缩因子(PF)和1.05 m L的消耗指数。发现预浓缩效率(PE)为9.55min〜(-1)。该方法成功用于水和尿液中钴的富集和测定,回收率令人满意。

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