电感耦合等离子体质谱法测定水泥中11种组分

采用7mL王水-2mL氢氟酸-2mL高氯酸-5mL硝酸体系对样品进行处理,选用⁴⁵Sc为内标校正²⁷Al、⁴⁷Ti、²⁴Mg、³⁹K和⁴³Ca,选用⁷²Ge为内标校正⁵⁷Fe、⁵³Cr、⁵⁵Mn和⁶³Cu,选用¹⁰³Rh校正²⁰⁸Pb和¹¹¹Cd,建立了电感耦合等离子体质谱法(ICP-MS)测定水泥中氧化铝、二氧化钛、氧化铁、氧化镁、氧化钾、氧化钙、铅、镉、铬、锰、铜等11种组分的方法。实验表明,在样品中加入7mL王水和2mL氢氟酸,置于80℃电加热装置上预处理20min,放入微波消解仪中进行消解,消解后样液中加入2mL高氯酸于160℃进一步消解样品并驱除多余的氢氟酸,再加入5mL硝酸驱除多余的高氯酸,可将样品溶解完全。在选定的实验条件下,各组分相应校准曲线的相关系数均不小于0.9996。按照实验方法对两种水泥标准物质GBW 03204b和GBW 03203b中的11种组分分别进行了8次平行测定,并分别加入铅、镉、铬、锰、铜的单元素标准溶液进行加标回收试验,所有组分测得结果的相对标准偏差(RSD,n=8)在3.7%~6.2%之间,氧化铝、二氧化钛、氧化铁、氧化镁、氧化钾、氧化钙的测定值与认定值基本一致,铅、镉、铬、锰、铜的加标回收率在87%~109%之间。

Determination of eleven components in cement by inductively coupled plasma mass spectrometry

The sample was treated in the system containing 7mL of aqua regia, 2mL of hydrofluoric acid, 2mL of perchloric acid and 5mL of nitric acid. ⁴⁵Sc was selected as internal standard to correct ²⁷Al, ⁴⁷Ti, ²⁴Mg, ³⁹K and ⁴³Ca; ⁷²Ge was selected as internal standard to correct ⁵⁷Fe, ⁵³Cr, ⁵⁵Mn and ⁶³Cu; ¹⁰³Rh was selected as internal standard to correct ²⁰⁸Pb and ¹¹¹Cd. A determination method of eleven components in cement (including aluminum oxide, titanium dioxide, iron oxide, magnesium oxide, potassium oxide, calcium oxide, lead, cadmium, chromium, manganese and copper) by inductively coupled plasma mass spectrometry (ICP-MS) was established. The experiments showed that the sample could be completely dissolved under the following conditions: 7mL of aqua regia and 2mL of hydrofluoric acid were added into sample; after pretreatment on electric heater at 80℃ for 20min, the sample was digested in microwave digestion system; then 2mL of perchloric acid was added into sample solution for further digestion at 160℃; after removing excessive hydrofluoric acid, 5mL of nitric acid was added to remove excessive perchloric acid. Under the selected experimental conditions, the correlation coefficients of calibration curves of components were all not less than 0.9996. Eleven components in two kinds of certified reference materials of cement (GBW 03204b and GBW 03203b) were determined for eight parallel times according to the proposed method. Meanwhile, the single-element standard solution of lead, cadmium, chromium, manganese and copper was added for recovery test. The relative standard deviations (RSD, n=8) of determination results were between 3.7% and 6.2%. The determination results of aluminum oxide, titanium dioxide, iron oxide, magnesium oxide, potassium oxide and calcium oxide were basically consistent with the certified values. The recoveries of lead, cadmium, chromium, manganese and copper were between 87% and 109%.