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| Optimization of ICP-OES pretreatment method for determination of Co content in Co-based catalysts for Fischer-Tropsch synthesis based on Response Surface Center Composite Design |
| Received:August 08, 2022 Revised:August 22, 2022 |
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| DOI：doi:10.3969/j.issn.2095-1035.2023.05.013 |
| KeyWord:ICP-OES; response surface method; center composite design; wet digestion; solid catalyst；Co |
| Author | Institution |
| JIANG Zhihui |
北京低碳清洁能源研究院 |
| ZHAO shuai |
北京低碳清洁能源研究院 |
| LIU congyun |
北京低碳清洁能源研究院 |
| MA Linge |
北京低碳清洁能源研究院 |
| LONG yinhua |
北京低碳清洁能源研究院 |
| Li yonglong |
北京低碳清洁能源研究院 |
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| Abstract: |
| To improve the accuracy of the determination of Co content in cobalt-based Fischer-Tropsch synthesis catalyst by inductively coupled plasma emission spectrometer (ICP-OES), the Response Surface Method Center Composite Design (RSM CCD) combined with single factor was used to optimize the pretreatment process for determination of Co content in Co-based catalysts for Fischer-Tropsch synthesis by the Inductively Coupled Plasma Optical Emission Spectrometer (ICP-OES). Three main parameters, i.e the acid ratio (VHCl：V(HCl+HNO3)), acid dosage, and temperature were considered in RSM. The relative error δ between the measured value of Co content and the true value and pretreatment time were selected as response of design. The optimum conditions were determined using statistical analysis and analysis of variance (ANOVA). The results showed that the theoretical δ was 0.001%, with the confidence interval at [0, 0.297] and digestion time was 0.57h, confidence interval was [0, 1.21] under the optimum condition. The amount of acid was obtained to be 10.6 mL in optimum condition and the best ratio and temperature were 0.44 and 180℃. Both δ and time fall within the confidence interval of the theoretical value through verification tests. The analysis results obtained by RSM were reasonable and feasible. In general, a simple, fast, high-accuracy and repeatable determination can be achieved by optimizing the experimental factors. |
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