Determination of eight elements in wet-process phosphoric acid by inductively coupled plasma atomic emission spectrometry
LONG Guang-hua1, MEI Yi*1, YANG Jia-qiang1, YU Bao-gen1, ZHANG Wen-li2
1. Faculty of Chemical Engineering, Kunming University of Science and Technology, Kunming 650093, China; 2. Key Laboratory for Nonferrous Vacuum Metallurgy of Yunnan Province, Kunming 650093, China
Abstract：The sample was dissolved with mixed acid composed by nitric acid and hydrochloric acid. 5%(V/V) hydrochloric acid was used as diluted acid. The sample solution was uniformly mixed by ultrasonic oscillation. The influence of matrix effect was eliminated by preparing the calibration curve with matrix matching method. Thus, a determination method of aluminum, magnesium, iron, potassium, sodium, calcium, manganese and chromium in wet-process phosphoric acid by multi-directional observation-inductively coupled plasma atomic emission spectrometry (ICP-AES) was established. According to the selection principle of analytical lines as well as the detection range of testing elements, the spectral lines with no or low interference, symmetrical peak shape and high sensitivity were selected as the analytical lines. Aluminum, magnesium and iron with high content were determined by radial observation mode to reduce the sample dilution ratio and ionization interference. Manganese, calcium and chromium with relatively low content were determined by axial observation mode to improve the sensitivity. Potassium and sodium with relatively low content were determined by axial attenuation observation mode to reduce the spectral intensity. The mass concentration of test elements in certain range were linear to their corresponding emission intensity. The linear correlation coefficients of calibration curves were between 0.998 6 and 0.999 9. The detection limits of method were between 0.001 5 μg/mL and 0.009 1 μg/mL. The content of aluminum, magnesium, iron, potassium, sodium, calcium, manganese and chromium in two wet-process phosphoric acid samples was determined according to the experimental method. The relative standard deviations (RSD, n=12) of results were between 2.1% and 8.1%. Two wet-process phosphoric acid samples were determined by matrix matching method and standard addition method combined with ICP-AES respectively, and then compared with other chemical methods (wherein, iron was determined by phenanthroline colorimetry; aluminum was determined by fluoride replacement-EDTA titration without pre-separation; calcium was determined by potassium permanganate titration method; manganese was determined by ammonium persulfate-ferrous titration; potassium, sodium, chromium and magnesium were determined by flame atomic absorption spectrometry). The determination results of aluminum, magnesium, iron, potassium, sodium, calcium, manganese and chromium showed good agreement.
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