Experimental design in chemistry: A tutorial

Leardi, Riccardo

doi:10.1016/j.aca.2009.06.015

Cited by 594 publications

(363 citation statements)

References 11 publications

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“…According to the ANOVA results, most compounds presented the variables temperature and extraction time as the most significant in the statistical test. 15 In addition to ANOVA, a Pareto graph (Figure 2) was obtained, in which most of the compounds were found to be more strongly affected by the extraction temperature, considering a confidence interval of 95%. This was expected, since it is known that in the HD-SPME technique there is a competition between the volatilization of the analytes and adsorption/desorption, with a temperature increase favoring desorption and volatilization.…”

Section: Resultsmentioning

confidence: 99%

“…The results were as expected, with higher affinity of the more polar compounds for PA and the nonpolar ones for PDMS. [12][13][14][15][16][17][18] The fiber selection was based on the overall best performance (i.e., larger chromatographic peak areas). The selection of the PA fiber was consistent with the findings of Santos et al, 17 who conducted a study comparing PDMS and PA for the extraction of chlorobenzenes in soil using HS-SPME.…”

Section: Resultsmentioning

confidence: 99%

“…The experimental model with the orthogonal central composite design, 3 central points, was used to optimize the extraction time and temperature, and the desorption temperature. 15,16 The extraction temperature varied from 20 to 60 o C, the extraction time from 10 to 50 min with exposed fiber and desorption temperature from 230 to 270 o C. The distribution of the points employed was -α; -1; 0; 1; +α, where α = 1.667. These working ranges were based on previous studies with soil samples using HS-SPME.…”

Section: Extraction Methodsmentioning

confidence: 99%

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Evaluation of Benzene Derivatives Migration from Solid Residuals by Alternative Leaching Process Using HS‑SPME GC‑MS

Dognini

Madureira

2018

J. Braz. Chem. Soc.

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Solid residues generated by the petroleum industry are often classified as hazardous, in part due to the lack of adequate analytical methods for their characterization, given their gluey and highly viscous nature. In this study, an alternative to the method described by the United States Environmental Protection Agency (US EPA) method 1311, replacing the zero headspace extraction (ZHE) approach with solid-phase microextraction followed by analysis via gas chromatographymass spectrometry was developed, for the determination of aromatic chlorinated and nonchlorinated volatile organic compounds. The method was validated according to national and international regulations, with a working range of 2.00 to 90.00 μg L -1 and limit of detection varying from 0.12 to 0.41 μg L -1 . Spiked matrices were analyzed and recovery values ranged from 79.7 to 98.4%. The analysis of real samples revealed levels below limit of quantification for chlorobenzene derivatives (2.00 μg L -1 ) and for the non-chlorinated aromatic compounds < 19.85 μg L -1, proving to be a viable alternative to overcome the difficulties encountered with filtration techniques.

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Section: Resultsmentioning

confidence: 99%

Section: Resultsmentioning

confidence: 99%

Section: Extraction Methodsmentioning

confidence: 99%

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Evaluation of Benzene Derivatives Migration from Solid Residuals by Alternative Leaching Process Using HS‑SPME GC‑MS

Dognini

Madureira

2018

J. Braz. Chem. Soc.

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“…The DoE is known to reduce the number of required experiments and to increase the quality of information simultaneously [32], since different factors vary on different levels at the same time. Nevertheless, the application of the DoE is largely unused in the field of methanation or catalyst activation by today.…”

Section: Design Of Experiments (Doe)mentioning

confidence: 99%

Low‐Temperature CO Methanation in Oil‐Tempered Plate Reactors by Optimization of Catalyst Activation Conditions

et al. 2017

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Ni-catalyzed methanation has been discovered more than 100 years ago. Since then, many applications based on syngas -from coal or biomass -for the production of synthetic natural gas (SNG) have been established. Nevertheless, methanation still bears great potential for optimization. Especially for decentralized, biomass-based applications, decreased methanation temperatures and pressures are expected to lower the costs of the overall process. Consequently, it is necessary to obtain a catalyst that is highly active under such reduced reaction conditions. This objective was successfully reached by a systematic variation of reduction temperature, pressure, and hydrogen concentration under the aspects of the design of experiment within the catalyst activation process.

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“…There are many types of experimental design techniques such factorial design (Full and Fractional Factorial Design), response surface methodology (Central Composite Design, Box-Behnken Design, Doehlert Design), Plackett-Burman Design, Mixture Design, Taguchi Design, etc [13]. In a Full Factorial Design, coefficient of linear interactions, two-term and three-term interactions can be examined [14]. However, full factorial experiments cannot always be conducted because of economy, time, or other constraints [15].…”

Section: Introductionmentioning

confidence: 99%

PREPARATION OF TiO2/PERLITE COMPOSITES BY USING 23-1 FRACTIONAL FACTORIAL DESIGN

Duranoğlu¹

2016

J. Turk. Chem. Soc., Sect. A: Chem.

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Successive impregnation and calcination processes were performed in order to produce TiO2/perlite composites. 2 3-1 fractional factorial design was first applied to optimize the production conditions of TiO2/perlite photocatalysts. Seven TiO2/perlite composites (including three central point experiments) were produced by manipulating three process parameters (amount of TiO2 used in impregnation process, particle size of perlite and calcination temperature). Prepared TiO2/perlite photocatalysts were characterized by XRay Diffraction Spectrometry and SEM. XRD patterns indicated that anatase was the main crystalline phase for all produced samples. Degradation capacities of produced TiO2/perlite composites were investigated in methylene blue degradation process. The linear models of TiO2 loading (%) and methylene blue degradation (%) of TiO2/perlite composites were developed by regression analysis of the experimental data. As a result of analysis of variance, it was found that developed models were statistically significant with the p-value of 0.0040 and 0.0003, for TiO2 loading (%) and methylene blue degradation (%), respectively. According to the coefficient of determination (0.9821 and 0.9970 for the models of TiO2 loading and methylene blue degradation, respectively) and error analysis, developed models fit well to the experimental data. Effect of process parameters was investigated by using response surface plots. Amount of TiO2 and particle size were found as the most effective parameters on both TiO2 loading (%) and degradation efficiency (%). Calcination temperature did not affect TiO2 loading but methylene blue degradation capacity.

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Experimental design in chemistry: A tutorial

Cited by 594 publications

References 11 publications

Evaluation of Benzene Derivatives Migration from Solid Residuals by Alternative Leaching Process Using HS‑SPME GC‑MS

Evaluation of Benzene Derivatives Migration from Solid Residuals by Alternative Leaching Process Using HS‑SPME GC‑MS

Low‐Temperature CO Methanation in Oil‐Tempered Plate Reactors by Optimization of Catalyst Activation Conditions

PREPARATION OF TiO2/PERLITE COMPOSITES BY USING 23-1 FRACTIONAL FACTORIAL DESIGN

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