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| Quantitative determination of Fe3O4, Fe2O3 and SiO2 in iron ore by Si internal standard-X-ray diffraction method |
| Received:July 18, 2022 Revised:August 09, 2022 |
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| DOI：doi:10.3969/j.issn.2095-1035.2023.05.009 |
| KeyWord:iron ore; phase; quantitative analysis; internal standard method; x-ray diffraction(XRD) |
| Author | Institution |
| QIAO Zhu |
连云港海关综合技术中心 |
| ZHENG Jianming |
南京海关工业产品检测中心 |
| SONG Jianfeng |
江苏沙钢集团有限公司 |
| ZHU Xiaodong |
上海思百吉仪器系统有限公司 |
| FENG Yahui |
南京海关工业产品检测中心 |
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| Abstract: |
| Accurate phase quantification of iron ore plays an important role in mineral value evaluation and mining and processing research. The existing chemical testing process is complicated and inefficient, and the X-ray Diffraction Rietveld Refinement Method is of poor traceability and difficult to evaluate and verify the accuracy of results. A method for quantitative determination of Fe3O4, Fe2O3 and SiO2 in iron ore by using Si as internal standard and Cu target X-ray as radiation source was established in the study. The diffraction spectrum was obtained by step scanning method. The calibration curve was established with the content of the measured phase as the abscissa and the peak area ratio of the measured phase to the internal standard phase as the ordinate. The sample preparation conditions, scanning parameters, internal standard selection, integration method, and overlapping peak correction were optimized in the experiment. The results showed that all the samples passed the 45 μm standard sieve. The proportion of Si internal standard was 10 %, the step length was 0.01°, and the step time was 30 S. The integral strength of the diffraction peaks of Fe3O4(311), Fe2O3(104), SiO2(011) and Si(111) was calculated, and the optimized results were obtained. Under the selected working conditions, the linear correlation coefficient (R2) of Fe3O4 in the range of 1.07 ~ 100 % was 0.9953, the relative standard deviation(RSD) was 1.1 % ~ 13.2 % (n=6), the recovery rate was 99.7 % ~ 114.8 %, and the detection limit (LOD) was 4.29 %. The linear correlation coefficient (R2) of Fe2O3 in the range of 1.51 ~ 100 % was 0.9991, the relative standard deviation(RSD) was 2.8 % ~ 10.6 %(n=6), the recovery rate was 87.1 % ~ 112.2 %, and the detection limit (LOD) was 2.56 %. The linear correlation coefficient (R2) of SiO2 was 0.9957 in the range of 0.79 ~ 29.72 %. |
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