CAJ | 학술논문

建立了铅试金富集-塞曼石墨炉原子吸收光谱法测定矿石样品中铂、钯、铑、铱的新方法.运用传统的铅试金方法熔融分解矿石样品,且采用留铅灰吹的方法使样品中铂、钯、铑、铱富集在约3 mg的铅合粒中.先用HNO_3溶解铅合粒,再加入HCl以形成王水溶解,使铂、钯、铑、铱完全进入溶液,然后采用塞曼石墨炉原子吸收光谱法于选定的仪器参数条件下测定.本方法运用二次方程最小二乘法拟合校准曲线,曲线拟合良好.铂、钯、铑、铱的校准曲线拟合系数分别为0.999 9、0.999 9、0.999 2、0.999 4;特征浓度分别为1.854 2 ng/mL、1.543 5ng/mL、0.488 3 ng/mL、0.481 1 ng/mL;相对标准偏差为:Pt 1.5%～4.5%、Pd 1.1%～2.9%、Rh 3.4%～6.3%、Ir 2.9%～5.8%.运用本方法测定标准物质中铂、钯、铑、铱含量,测定结果与认定值相吻合.
건립료연시금부집-새만석묵로원자흡수광보법측정광석양품중박、파、로、의적신방법.운용전통적연시금방법용융분해광석양품,차채용류연회취적방법사양품중박、파、로、의부집재약3 mg적연합립중.선용HNO_3용해연합립,재가입HCl이형성왕수용해,사박、파、로、의완전진입용액,연후채용새만석묵로원자흡수광보법우선정적의기삼수조건하측정.본방법운용이차방정최소이승법의합교준곡선,곡선의합량호.박、파、로、의적교준곡선의합계수분별위0.999 9、0.999 9、0.999 2、0.999 4;특정농도분별위1.854 2 ng/mL、1.543 5ng/mL、0.488 3 ng/mL、0.481 1 ng/mL;상대표준편차위:Pt 1.5%～4.5%、Pd 1.1%～2.9%、Rh 3.4%～6.3%、Ir 2.9%～5.8%.운용본방법측정표준물질중박、파、로、의함량,측정결과여인정치상문합.
A novel method for determining platinum palladium, rhodium and irdium in mineral sample was established using Zeeman graphite furnace atomic absorption spectrometry. Mineral sample was melten using traditional lead fire assaying, and platinum, palladium, rhodium and irdium was accumu-lated in 3 mg of lead by cupellation. This alloy was dissolved in HNO_3, and then HCI was added to form aqua regia solution to make sure that platinum, palladium, rhodium and irdium were fully dis-solved in this solution. The concentration of the above four elements was detected at the selected in-strumental parameters using Zeeman graphite furnace atomic absorption spectrometry. A calibration curve was created based on linear least squares fitting technique with a satisfactory curve fitting effect. The standard correlation coefficients are 0.999 9, 0.999 9, 0.999 2 and 0.999 4,and the characteristic concentration is 1.854 2 ng/mL, 1.543 5 ng/mL, 0. 488 3 ng/mL, and 0. 481 1 ng/mL for platinum, palladium, rhodium and irdium, respectively. The relative standard deviations (n=4) are 1.5%-4.5% (Pt), 1.1%-2.9% (Pd), 3.4%-6.3% (Rh), 2.9%-5. 8% (Ir). The concentration of plat-inum, palladium, rhodium and irdium of standards material detected by this method is consistent with the certified value.