Determination of titanium, zirconium, aluminum and calcium in metallocene catalyst by inductively coupled plasma atomic emission spectrometry after pressure digestion
RONG Li-li1, ZHANG Yan1, ZHAO Tie-kai1, ZHANG Shu-quan2, SUN Ling1
1. Daqing Chemical Engineering Research Center,PetroChina Petrochemical Research Institute,Daqing 163714, China; 2. PetroChina Daqing Petrochemical Company,Daqing 163711,China
Abstract：The metallocene catalyst was treated using 3.0mL of HCl, 2.0mL of HNO3 and 4.0mL of HF by high-pressure digestion technique to prepare sample solution. Ti 334.940nm, Zr 343.823nm, Al 396.153nm and Ca 317.933nm were selected as the analytical lines. The determination method of Ti, Zr, Al and Ca in metallocene catalyst by inductively coupled plasma atomic emission spectrometry (ICP-AES) was established. The content of Al in solution was relatively high and greatly influenced on the determination of Ti, Zr and Ca. In and Cs were selected as internal standard elements in experiments to eliminate the matrix interference. For the sample with high content Al, the solution should be firstly diluted before determination. The content of Ti, Zr and Ca could be directly determined by on-line adding In internal standard solution. The correlation coefficients of calibration curves of elements were higher than 0.9998. The precision test was conducted using a metallocene catalyst sample, and the relative standard deviations (RSD, n=6) of found results were less than 1.7%. The experimental method was applied for the determination of metallocene catalyst sample. The results were consistent with those obtained by ICP-AES after sampel treatment by microwave digestion.
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