Determination of eleven components in cement by inductively coupled plasma mass spectrometry
ZHANG Cui-xin1, YAO Chun-yi*2, JU Jing-ya2, DONG Ya-nan1, MA Ying-nan2
1. Hebei Research Institution for Product Quality Supervision and Inspection, Shijiazhuang 050227, China; 2. Hebei Entry-exit Inspection and Quarantine Technical Center, Shijiazhuang 050051, China
Abstract：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%.
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