CAJ | 학술논문

建立了密闭溶样-电感耦合等离子体质谱法同时测定煅烧高岭土中铜、铅、锌、铬、镉和锰等6个微量重金属元素的有效方法.实验中对仪器的最佳工作参数进行了优化,选择适当的同位素,并用铑作内标元素,有效地抑制了分析信号的漂移以及分子和多原子离子的质谱干扰;探讨了混合酸消解体系、消解液用量、密闭溶样的时间对测定结果的影响.以硝酸-氢氟酸作为消化试剂,在180℃下溶解4 h能完全消解样品.在选定的实验条件下,对煅烧高岭土样品进行了精密度和回收率试验,方法相对标准偏差(RSD,n=9)为0.96%～2.22%,加标回收率为98.0%～101.5%.
건립료밀폐용양-전감우합등리자체질보법동시측정단소고령토중동、연、자、락、력화맹등6개미량중금속원소적유효방법.실험중대의기적최가공작삼수진행료우화,선택괄당적동위소,병용로작내표원소,유효지억제료분석신호적표이이급분자화다원자리자적질보간우;탐토료혼합산소해체계、소해액용량、밀폐용양적시간대측정결과적영향.이초산-경불산작위소화시제,재180℃하용해4 h능완전소해양품.재선정적실험조건하,대단소고령토양품진행료정밀도화회수솔시험,방법상대표준편차(RSD,n=9)위0.96%～2.22%,가표회수솔위98.0%～101.5%.
A method for the determination of copper, lead, zinc, chromium, cadmium and manganese in calcined kaoline samples by inductively coupled plasma-mass spectrometry (ICP-MS) with pressurized acid digestion was developed. The ICP-MS instrument operating parameters were optimized. The mass spectral interferences were eliminated by selecting ~(65)Cu, ~(208)Pb, ~(66)Zn, ~(52)Cr, ~(114)Cd and ~(55)Mn as analytical isotopes. And Rh was selected as internal standard to compensate the analytical signal drift. The factors affecting the analytical results such as selection of sample digestion system, dosage of the digestion solvents and digestion time were studied. Under the optimized condition with HNO_3-HF digestion system at 180℃ for 4 h, the recovery for these elements was 98.0%～101.5% with precision of 0.96%～2.22%RSD(n=9). The proposed method has been applied to the determination of these trace heavy metal elements in calcined kaoline samples with satisfactory results.