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为了防止稀土的低附加值滥用,控制陶瓷色釉料中的稀土含量尤为重要,本方法为制订出入境检验检疫行业标准《陶瓷色釉料中稀土总量的测定电感耦合等离子体原子发射光谱法》提供可靠依据。由于陶瓷色釉料极其稳定的化学性质,因此不能采用传统的消解方法进行样品前处理,本文提出了用改进后的氢氧化钠和过氧化钠体系高温碱熔陶瓷色釉料,再用电感耦合等离子体原子发射光谱仪测定La,Ce,Pr,Nd,Sm,Eu,Gd,Tb,Dy,Ho,Er,Tm,Yb,Lu,Y 15种稀土元素总量的方法。在陶瓷色釉料的消解方法、待测元素波长的选择和基体干扰校正方面进行重点研究。选取具有代表性的陶瓷色釉料样品进行回收率、精密度及重现性试验,测得方法的回收率在94.7%~102.7%,精密度小于2.7%,重现性小于4.3%。计算了15种稀土元素的检出限均小于0.51 mg·kg-1。
In order to prevent the misuse of low added value of rare earth, the control of rare earth content of ceramic glaze is particularly important, this method is to develop entry-exit inspection and quarantine standards “Determination of total rare earths in ceramic color glaze inductively coupled plasma atomic emission spectrometry ”Provide a reliable basis. Because of the extremely stable chemical properties of ceramic color glaze, the traditional digestion method can not be used for sample pretreatment. In this paper, high temperature alkali-melting ceramic color glaze with improved sodium hydroxide and sodium peroxide system, Determination of total rare earth elements in La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu and Y by coupled plasma atomic emission spectrometry. In the ceramic color glaze digestion method, the choice of the wavelength of the selected elements and matrix interference correction focus. The representative samples of ceramic glaze samples were selected for recovery, precision and reproducibility. The recoveries of the methods were 94.7% -102.7%, the precision was less than 2.7% and the reproducibility was less than 4.3%. The calculated limits of detection for 15 rare earth elements were all less than 0.51 mg · kg-1.