首页> 外文期刊>Journal of Geology and Mining Research >Application of two-level full factorial design and response surface methodology in the optimization of inductively coupled plasma-optical emission spectrometry (ICPOES) instrumental parameters for the determination of platinum
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Application of two-level full factorial design and response surface methodology in the optimization of inductively coupled plasma-optical emission spectrometry (ICPOES) instrumental parameters for the determination of platinum

机译:二级全因子设计和响应面方法在优化电感耦合等离子体发射光谱法(ICPOES)测定铂的仪器参数中的应用

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Inductively coupled plasma optical emission spectrometry (ICP-OES) determination of platinum was optimized using 2-level, 4-factor full factorial design and response surface methodologies. Four factors, namely carrier gas flow rate, sample solution flow rate as represented by the pump speed, plasma observation height and RF power, were employed in the factorial design. Analysis of variance (ANOVA) at a p-value significance level of 0.05 was used to assess the significance of the factors on platinum analytical line emission intensity. The main effects of carrier gas flow rate and plasma power, and the interaction effect of carrier gas flow rate and plasma power, were found to be statistically significant and were varied during subsequent optimization procedure using contour map and response surface methodologies. Plasma observation height and pump speed were found to have an insignificant effect on the platinum intensity and were held constant at 10 mm above the load coil and 30 revolutions per minute, respectively during the optimization procedure. The optimized procedure comprised of a carrier gas flow rate of 0.70 L/min and plasma power of 1400 W, and was validated by analysis of Certified Reference Materials (CRMs) AMIS 0132 for low platinum grades and AMIS 0164 for high platinum grades. The instrumental limit of detection (LOD) and limit of quantization (LOQ) obtained were 0.035 µg/g Pt and 0.105 µg/g Pt, respectively, and highly precise determinations of Pt (0.21 to 0.24% RSD) were obtained when three batches of PMG ore floatation concentrates were analyzed using the optimized ICP-OES parameters.
机译:电感耦合等离子体发射光谱法(ICP-OES)使用2级,4因子全因子设计和响应面方法对铂的测定进行了优化。析因设计中采用了四个因素,即载气流速,以泵速表示的样品溶液流速,血浆观察高度和RF功率。 p值显着性水平为0.05的方差分析(ANOVA)用于评估因素对铂分析线发射强度的显着性。发现载气流速和等离子功率的主要影响以及载气流速和等离子功率的相互作用具有统计学显着性,并且在随后的优化过程中使用等高线图和响应面方法进行了变化。发现等离子体观察高度和泵浦速度对铂强度没有显着影响,在优化过程中,等离子体观察高度和泵浦速度分别保持恒定在负载线圈上方10 mm和每分钟30转。优化的程序包括0.70 L / min的载气流量和1400 W的等离子功率,并通过对低铂金等级的认证参考材料(CRM)AMIS 0132和对高铂金等级的AMIS 0164的分析进行了验证。仪器的检测限(LOD)和定量限(LOQ)分别为0.035μg/ g Pt和0.105μg/ g Pt,并获得了高精度的Pt测定(0.21至0.24%RSD)。使用优化的ICP-OES参数分析了三批PMG矿石浮选精矿。

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