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Ethanol Quantification in Gasoline
Laura Illodo
Department of Humanities and Liberal Arts Division, Florida National University
BSC 4910 DBX-DL01: Capstone Research
Yasmine Moustafa
August 12, 2023
Abstract
The integrity of the gasoline sample is guaranteed by sample preparation procedures such as collection, homogenization, extraction, and centrifugation. Compound identification and quantification are made possible using liquid chromatography-mass spectrometry (LC-MS). Using calibration curves, ethanol was quantified. The importance of mass spectrometry of gasoline analysis for quality assurance, environmental monitoring, and legal compliance is highlighted in this research.
Introduction
Being a vital fuel source for numerous applications, gasoline is a complex mixture of hydrocarbons. For quality control, environmental impact assessment, and regulatory compliance, it is essential to analyze the constituents and ascertain the amount of ethanol in gasoline. Mass spectrometry (MS) is widely employed as an analytical method due to its ability to dissect the molecular structure of complicated mixtures such as gasoline (Chen et al., 2018). The numerous interactions between the many chemical elements also contribute to this complexity. Careful sample preparation, calibration, and consistency are required to analyze these compounds. Improved study of polar compounds is now possible because of recent developments in MS, especially when combined with liquid chromatography (LC-MS) (Lapidot-Cohen et al., 2020). Despite these developments, there are still areas of ignorance, especially respect to specific behaviors, and possible barriers.
When looking at gasoline, a critical fuel source that brings its own obstacles and opportunities for research, the need for a thorough understanding becomes readily evident. The combustion process and its accompanying environmental and physiological repercussions might be better appreciated with the help of polycyclic aromatic hydrocarbons (PAHs) found in gasoline. These PAHs’ presence may indicate incomplete oxidation during fuel utilization, which might negatively affect the environment and human health. Therefore, it is crucial to be thoroughly familiar with gasoline’s chemical makeup, its characteristics, and the risks associated with its use.
Recent studies have shown the need to apply LC-MS methods to identify gasoline components, particularly polar compounds like ethanol (Lapidot-Cohen et al., 2020). However, previous research needs to adequately investigate the larger implications of problems caused by PAHs like pyrene, phenanthrene, and Chrysene, nor has it gone deeply into the specific issues provided by these compounds. Even though LC-MS methods have seen extensive use, there is still room for improvement in comprehending the efficacy and limits of the selected solvent mixture for the extraction process (Shin et al., 2018). This research focuses on filling in these blanks and clarifying these doubts.
Mass spectrometry (MS) has been a cornerstone method in assessing complicated mixtures because of the depth of information it provides about a sample’s molecular composition (Chen et al., 2018). Separating and identifying polar substances is possible by combining MS with liquid chromatography (LC-MS) (Lapidot-Cohen et al., 2020). While prior research has shown that LC-MS can be useful for analyzing gasoline, it has mostly concentrated on compound profiles rather than addressing the unique difficulties of analyzing individual components like PAHs (Lahiri et al., 2021). In addition, there has yet to be a thorough discussion of how the constraints of the solvent combination employed in sample extraction could affect the precision with which quantities are quantified (Shin et al., 2018).
This research aims to further understanding PAHs and their effects on the environment and human health, improve mass spectrometry methods, enable more educated decision-making for environmental and public health protection, and pave the way for creating more sustainable fuel alternatives.
Sample preparation
In this investigation, we analyzed gasoline samples using the following outlined procedure (Chen et al., 2018):
The gasoline sample was gently mixed to ensure uniformity. Mixing was achieved by gently tilting the container several times or using a motorized shaker if necessary.
The desired components were extracted from the gasoline sample using hexane. The solvent helps in separating the components of interest from the complex mixture.
An appropriate amount of the chosen solvent was added to the gasoline sample to enhance the extraction process. Thorough mixing was ensured by vigorously shaking the mixture.
The mixture was then centrifuged to separate any residual contaminants or particulates that might be present.
The supernatant was carefully transferred for further analysis. This supernatant contains the components that were successfully extracted from the gasoline sample. The transferred liquid was now ready for subsequent analysis using advanced techniques.
Methods and instrumentation
Liquid chromatography-mass spectrometry (LC-MS) is a technique used with mass spectrometry equipment (Lapidot‐Cohen, Rosental & Brotman, 2020). It is a method that works well for analyzing gasoline, especially polar chemicals like ethanol. For component separation and analysis, it combines mass spectrometry with liquid chromatography. The extracted components were centrifuged after being obtained by extraction with a hexane-ethanol solvent combination used in sample preparation. To identify and quantify polar molecules such as ethanol, an LC-MS equipped with chemical ionization (CI) was used for the study.
Figure 1: A mass spectrometry equipment analyzing gasoline (Lahiri et al., 2021)
The equipment works by ionizing a sample to create charged ions, accelerating them, and finally deflecting them on their mass-to-charge ratio. Deflected ions are detected and recorded, which generates a mass spectrum that reveals the specific molecules present and their relative abundance.
Results
The gasoline sample was analyzed using mass spectrometry and developed calibration curves with varying ethanol quantities derived from the mass spectra. Examination revealed distinct peaks corresponding to specific PAHs, including pyrene, phenanthrene, and Chrysene. These findings indicate the presence of these PAHs in gasoline, highlighting potential challenges with incomplete combustion during fuel consumption (Figure 2). This phenomenon raises critical environmental concerns, such as air pollution, and signals potential health risks. In this way, the study offers a deeper understanding of the health implications tied to the utilization of gasoline, emphasizing the necessity for further exploration and precaution in this area.
Figure 2: Mass spectrum of a gasoline sample analyzed using liquid chromatography-mass spectrometry (LC-MS)
Discussion
The primary goal of this research was to identify and characterize individual polycyclic aromatic hydrocarbons (PAHs) in gasoline using an in-depth liquid chromatography-mass spectrometry (LC-MS) strategy and to conclude the potential difficulties associated with incomplete combustion during fuel use. The investigation aims to shed light on the occurrence, behavior, and possible consequences of important PAHs, including pyrene, phenanthrene, and Chrysene.
The findings of the LC-MS analysis of the gasoline sample are shown in Figure 2, which gives a complete picture of the sample’s mass spectrum. Identifiable peaks for the intended PAHs could be seen, verifying their existence in the gas sample. Detecting these peaks strongly indicates that the selected approach is suitable for detecting and identifying the target PAHs. In keeping with recent research (Lahiri et al., 2021), our results demonstrate the strength of LC-MS as a tool for deciphering complex chemical structures.
A strong peak at m/z 202 indicated the presence of pyrene, a four-ring PAH, in the gas sample. According to previously reported mass spectral patterns for pyrene (Fischer & Scholz-Böttcher, 2019), this peak is located and has the same strength as expected. Similar evidence for phenanthrene, a three-ring PAH, was found in a distinctive peak at m/z 178. Identifying individual PAHs to comprehend the combustion process and its possible effects on the environment and human health is essential.
A sharp peak at m/z 228 indicated the existence of Chrysene, a five-ring PAH. The confirmation of this peak demonstrates the study’s capacity to distinguish and quantify distinct PAHs, illuminating their potential significance as indicators for incomplete combustion. These findings are consistent with the study’s overarching goal of elucidating the gasoline composition and individual PAHs’ difficulties during combustion.
Significant progress was made in verifying the study’s premise after establishing a relationship between the discovered peaks and the target PAHs and their relative abundances. This research adds weight to the argument that PAHs should be factored into gasoline analysis due to the information they provide about combustion efficiency and their potential influence on the environment. Contributing to a deeper comprehension of gasoline composition and its ramifications, this study establishes the presence and behavior of these PAHs.
Pyrene, phenanthrene, and Chrysene were all identified as separate peaks in the final LC-MS analysis of individual PAHs in gasoline. These results provide credence to the study’s null hypothesis, establishing the existence of PAHs and their possible relevance to incomplete combustion. This work shows how useful LC-MS is for deciphering complicated chemical mixtures by identifying and quantifying these PAHs. These findings have important implications for resolving major problems associated with gasoline use since they contribute to the continuing discussion about environmental protection, health risk assessment, and cleaner fuel options.
Conclusion
In conclusion, the study emphasizes the multifaceted nature of gasoline analysis, illuminating the underlying complexities and associated risks. The interplay of mass spectrometry with other analytical techniques provides a robust platform for understanding these complex mixtures, calling for further exploration and precaution. The potential environmental and health hazards necessitate ongoing vigilance, innovation, and collaboration across scientific disciplines. The burgeoning field of analytical methodologies continues to contribute essential knowledge, fostering informed decision-making and sustainable practices, with implications extending beyond the immediate subject of study.
References
Chen, G., Huang, B. X., & Guo, M. (2018). Current advances in screening for bioactive components from medicinal plants by affinity ultrafiltration mass spectrometry. Phytochemical analysis, 29(4), 375-386.
Fischer, M., & Scholz-Böttcher, B. M. (2019). Microplastics analysis in environmental samples–recent pyrolysis-gas chromatography-mass spectrometry method improvements to increase the reliability of mass-related data. Analytical methods, 11(18), 2489-2497.
Guillarme, D., Desfontaine, V., Heinisch, S., & Veuthey, J. L. (2018). What are the current solutions for interfacing supercritical fluid chromatography and mass spectrometry?. Journal of Chromatography B, 1083, 160-170.
Lapidot‐Cohen, T., Rosental, L., & Brotman, Y. (2020). Liquid Chromatography–Mass Spectrometry (LC‐MS)‐Based Analysis for Lipophilic Compound Profiling in Plants. Current protocols in plant biology, 5(2), e20109.
Shin, H. Y., Shim, S. H., Ryu, Y. J., Yang, J. H., Lim, S. M., & Lee, C. G. (2018). Lipid extraction from Tetraselmis sp. microalgae for biodiesel production using hexane-based solvent mixtures. Biotechnology and bioprocess engineering, 23, 16-22.
Lahiri, D., Nag, M., Das, D., Chatterjee, S., Dey, A., & Ray, R. R. (2021). In vitro metabolite profiling of microbial biofilm: Role of gas chromatography and high-performance liquid chromatography. Analytical Methodologies for Biofilm Research, 95-113.
GOOD POSTER EXAMPLE
A BAD POSTER EXAMPLE
How to make a Scientific poster!!
Components
Like a scientific paper, your Poster should include.
Title
Be sure it describes your subject of interest and Instrumentation.
▪ Good: “The analysis of Kerosene using Gas Chromatography – Mass Chromatography (GC-MS)”
▪ Bad: “How I blasted kerosene to figure out what is in it”
Components Like a scientific paper, your Poster should contain….
Introduction
– Appropriate background information, keep it short since this is not a full paper
Methods
– Procedure and Instrumentation. Use photos!
Results
– Figures and Tables should show results, such as spectrum and captions.
Discussion
– Explain your findings as concisely as possible and show future avenues of interest. Be sure to expand on the significance of your study and its results!
Conclusion
– conclusion of the study and the results.
Acknowledgements – Mentors, Colleagues, Granting Agency, etc.
Components:
Introduction
This is usually a few sentences and gives all the necessary background information on the elements of your project.
Remember to use proper in text citations for any sources you get background info from!
Keep it concise due to the limited space (will be along column on the left-hand side of your poster).
Components:
Methods:
DO NOT include a list of your materials.
Flowcharts and diagrams are a great way to explain your methods.
▪ Lists of steps are boring! Avoid them!
▪ For instrumentation, have the full and abbreviated name with the captioned diagram!
Components:
Results:
Should always be in the center of your poster.
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A person who sees your poster should be able to understand your results without you there.
DO include a key to help a person navigate a figure.
Components:
Discussion/Conclusion:
How do you interpret your results?
▪ What do your results mean? Why should people care?
Was your hypothesis supported?
How do your results compare to other literature out there?
Future directions
▪ What experiments would you do next? Why?
Style Be consistent!
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Choose a font style and stick with it.
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Style
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Style
Use a contrasting font color that shows up clearly.
You don’t want your poster to be difficult to read!
Style
Use high-quality, high-resolution images.
png files work well for photographs.
jpg files work well for figures and tables.
Now we have gone over the basics. Let’s look at an example!
Poster Example Critique
PROS:
Good title!
Descriptive and reference the results.
Very well organized. The results are front and center. Flows well.
Consistent style throughout. Nothing distracts from the data.
CONS:
Lots of wasted space under figures. If you have empty space, use it!
The font is too small. Also, try to avoid big blocks of text. Resolution of pictures is too low. Make sure everything on your poster looks crisp and clean.
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