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Article

Compositional Analysis of Biodiesel Particulate Matter (BPM) from a Non-Road Diesel Generator

by
Mingming Lu
1,*,
Aisha Tzillah
1,
Ming Chai
2 and
Omer Aloraimi
1
1
Department of Chemical and Environmental Engineering, University of Cincinnati, Cincinnati, OH 45221, USA
2
American GreenFuels LLC, 30 Waterfront Street, New Haven, CT 06512, USA
*
Author to whom correspondence should be addressed.
Energies 2023, 16(13), 5010; https://doi.org/10.3390/en16135010
Submission received: 13 April 2023 / Revised: 19 June 2023 / Accepted: 24 June 2023 / Published: 28 June 2023
(This article belongs to the Special Issue Advances in Biodiesel for Application in Diesel Engines)
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Abstract

:
There have been multiple studies of biodiesel particulate matter (BPM) emissions over the years, but few are on non-road diesel engines despite their higher emissions and less regulation. The goal of this paper is to further investigate the impacts of biodiesel fuel on particulate matter emissions. Compositional analysis of BPM was performed on a non-road diesel generator under various loads using different diesel and biodiesel blends. In order to account for organic compositions from both petroleum diesel and biodiesel, two types of analytical columns were used, one for polar compounds such as fatty acid methyl esters (FAME) and another non-polar column for hydrocarbons and PAHs (polycyclic aromatic hydrocarbons). In the BPM emitted, FAME constituted 6% to 11% of the total mass at different loads, which is the highest among the soluble organic fractions. This is an indication that biodiesel fuel might not be completely combusted in this diesel engine. The PAH fraction of the B50 (50% biodiesel) is much less than that found in petroleum diesel PM (B0). The elemental carbon fraction of the B50 particulate matter is less than that from B0. The lower PAH and soot from biodiesel blends may correspond to lower toxicity.

1. Introduction

Since late 1990s, the production and consumption of methyl ester-based biodiesel have increased significantly around the world due to many desirable properties of biodiesel, such as being renewable, carbon neutral, less polluting, and compatibility with diesel fuel infrastructure, etc. For example, in the USA, biodiesel production has been steadily increasing for more than two decades and reached 1817 million gallons in 2020, making it the third largest biodiesel producer in the world only after Indonesia and Brazil. The USA’s biodiesel production capacity in 2022 was 2255 million gallons, with more than 50% originating in the Midwest of the USA and using soybean as the major feedstock [1].
Biodiesel is regarded as a drop-in solution to the problems caused by petroleum diesel. However, it constitutes less than 4% of diesel consumption in the USA. There is ample room for growth since low-level blends below B5 (5% biodiesel by volume) are considered diesel fuel with no need for separate labelling at the pump, and B20 is certified as safe to use by most original diesel engine manufacturers [2].
Brazil set its biodiesel blending target at B15 for 2023 [3] but recently reverted back to B10 in 2022 for economic reasons [4]. In order to reduce its carbon footprint, Indonesia is still committed to a blending mandate at B30 despite the higher cost of biodiesel [5], while Malaysia has set B10 as its blending target [6]. Biodiesel production in the European Union (EU) was 13 million tonnes in 2020 with a current permitted blending level of B7 [7].
While the transportation sector is moving toward electrification to decarbonize its light-duty fleets, diesel technologies are still needed for mid- to heavy-duty and off-road applications. Interests in biodiesel have recently expanded into locomotives and ships [8,9,10]. Since biodiesel is much more carbon neutral than petrol diesel [11], its use is expected to increase in the near future due to the transition to a carbon-neutral economy.
There have been multiple reports on air pollutant emissions using biodiesel blends over the years, with the majority of studies reporting less carbon monoxide, less particulate matter, and higher NOx emissions comparing with petroleum diesel [12,13,14,15]. Only a few studies have reported opposite trends in emissions [10]. People have come to realize that emissions are dependent on many factors, such as engine and feedstock specific conditions, engine operations, sample collection methods, etc.
However, very limited information is available with regard to the use of biodiesel blends in non-road diesel engines, despite the fact that non-road diesel engines tend to be much older and higher in quantity of emissions released. Non-road engines and on-road diesel engines respond differently to biodiesel blends, since non-road engines mainly operate in transient modes [13,16]. Studies on diesel particulate matter indicated that the compositions can be attributed to petrogenic sources, such as fuel evaporation and pyrogenic sources due to incomplete combustion. Although fuel compositions were found from DPM, fewer studies have reported FAME components from BPM that represent the impacts of biodiesel fuel.
The presence of methyl ester in BPM has been suggested by FTIR [17,18].TG-MS analysis of BPM filters identified fragments at m/z 294, 296, and 298, which represented the methyl ester components of biodiesel at C18:2, C18:1, and C18:0 respectively [17]. However, there have not been reports of individual FAME compositions in GC-MS studies, unlike those for diesel particulate matter. Part of the challenge may be the complexity of analysis, in that sample preparation and analysis are very different between polar FAME in biodiesel and non-polar hydrocarbons and PAHs.
Therefore, the purpose of this paper is to provide a detailed compositional analysis of particulate matter from biodiesel blends to fill in the gap in identifying individual FAME compositions via GC-MS. This article is the first one to employ two types of analytical columns for BPM compositional analysis. In addition, load-variated emissions of carbon monoxide, carbon dioxide, and nitrous oxides (NOx) and mass-based particulate matter were also presented. Carbon fractions of the BPM were investigated via OC/EC (organic/elemental carbon) analysis. Soluble organic fractions of the BPM were also studied by each compositional category.

2. Materials and Methods

On-road ultra-low sulfur diesel (ULSD) fuel with a sulfur content of less than 15 ppm (referred to as B0) was purchased from gas stations. B100 (100% biodiesel) was purchased (product name Nexsol Biodiesel) from a vender, while biodiesel blends, such as B50, were made in situ, consisting of 50% of biodiesel and 50% petroleum diesel by volume. HPLC grade dichloromethane (DCM) was purchased from Aldrich. The following standard reference compounds were acquired from Restek Corporation to quantify individual peaks eluted from GC-MS: a DRO mixture (Tennessee/Mississippi), catalogue number 31,214, for normal alkanes ranging from n-C10 to n-C25; a 16-PAH (polycyclic aromatic hydrocarbon) standard with catalogue number 31,011 SV Calibration Mix #5; and a methyl ester standard with catalogue number 35,024, AOCS Standard #3 Rapeseed Oil.
For this study, a non-road 4-stroke diesel engine generator (1992 Generac Model SD080) was utilized. It was a compression-ignition, direct-injection, turbo-charging, 4 cylinder engine and had a rated output of 80 kW, 60 Hz, with a normal engine speed of 1800 rpm and a compression ratio 17.5:1, and is not equipped with any emission control. At the time of testing, the generator had approximately 750 h of usage, far below its estimated 8000 h useful lifetime. All rubber tubing fuel lines in the engine were replaced with polyurethane tubing prior to biodiesel use. The exhaust pipe was extended to the ground for sample collection. A load simulator (Merlin 100, SIMPLX) was used to produce various load conditions from 0 (idle) to 75 kW at 25 kW increments by applying steady state banks of heaters to the generator. Three fuels were tested, neat biodiesel (B100), biodiesel blend (B50), and petroleum diesel (B0). Multiple measurements were taken at each load.
A schematic diagram of the sampling method with dimensions is shown in Figure 1, which has also been used in other studies [17,19]. A high-volume dilution sampler with a flow rate of approximately 300 L/min was employed. The slipstream of the engine exhaust was drawn into the sampler together with ambient air filtered using a high-efficiency particulate (HEPA) filter for dilution ratios of approximately 3.4. The total diluted sample flow rate was determined via a Magnehelic gauge, while the dilution air was measured with a Dwyer Ratemaster flow meter.
The PM was collected on 90 mm quartz fiber filters (Millipore) at temperatures less than 45 ± 5 °C, followed by a cartridge with PUF/XAD-2/PUF to remove semi-volatile compounds. The quartz fiber filters were baked at 550 °C for a minimum of 12 h prior to sampling. After sampling, the filter paper was put into a labeled petri dish and stored in a desiccator prior to analysis.
Gaseous emissions of carbon monoxide (CO), carbon dioxide (CO2), and oxides of nitrogen (NOx) were measured with a portable emission gas analyzer (Testo 350, West Chester, PA, USA).
A Varian GC/MS system (CP-3800 GC, Saturn 2200 Ion Trap MS) in selective ion search mode was used for analysis. Two analytical methods were developed to accommodate two distinct types of products, non-polar hydrocarbons and polar methyl esters, each requiring its own analytical column and sample preparation procedures.
After the PM mass was measured gravimetrically, the filter sample was extracted via DCM under sonication and was filtered to remove insoluble fractions. The solution was then split into two fractions; one fraction was concentrated to approximately 1 mL for hydrocarbon analysis, and the other unconcentrated fraction was used for methyl ester analysis.
Hydrocarbons such as alkanes and PAHs were analyzed with a non-polar column (CP-Sil 8 CB Low Bleed/MS, 30 m × 0.25 mm ID coating × 0.25 mm), which is equivalent to a DB-5ms capillary column. The MS spec detector was turned off at select times when the large DCM solvent peak and methyl ester peaks were expected to elute.
Methyl esters were analyzed with a polar CP Wax 58 (DB-FFAP equivalent) capillary column (Varian Inc., Palo Alto, CA, USA, 30 m × 0.32 mm × 0.25 mm). The effectiveness of the FAME analytical setup was verified with B100 fuel, and results were consistent with the certificate of analysis provided by the vendor [20].
The organic and elemental carbon (OC/EC) analysis was conducted using NIOSH method 5040, a thermal–optical transmittance method. Punches of 1.5 centimeters square were made on the BPM filter, which were then put into the OC/EC analyzer (Sunset Laboratories). The mass of this punch was measured before and after OC/EC analysis to obtain the BPM weight. OC and EC results for B0 and B50 and are expressed as % relative to the mass of the particulate matter. The non-carbonaceous fraction was determined by finding the difference.

3. Results and Discussion

3.1. Gaseous Emissions from B0, B50 and B100

Figure 2 illustrates gaseous emissions of carbon monoxide (CO), carbon dioxide (CO2), and nitrogen oxides (NOx) respectively. Lower carbon monoxide levels (Figure 2a) were observed in the neat biodiesel (B100) and biodiesel blend (B50) samples than in the petroleum diesel (B0) samples. B100 use resulted in the highest CO reduction, a 60% decrease at 0 kW and an 85% decrease at 75 kW compared with B0. CO emissions decreased with engine loads for all three fuels, which is likely due to greater air intake at higher loads. This is expected, as carbon monoxide results from incomplete combustion, which can be alleviated by the use of oxygenated fuels such as biodiesel. This is consistent with multiple studies such as [13,14,15].
As shown in Figure 2b, CO2 emissions increased with load and with biodiesel fractions. On average, a 20% increase was observed for B50, and a 30% increase for B100 when compared with B0. This is likely due to both the oxidation of the carbon chain and the decarboxylation of the methyl esters [21]. In addition, the fuel bound oxygen content in biodiesel can also reduce incomplete combustion in localized fuel-rich regions [22,23]. The CO2 increase with engine load is likely due to higher temperatures and higher fuel usage at higher loads [24].
NOx emissions in Figure 2c, however, were higher for B50 and B100 than B0, except B50 at 0 kW. B100 use resulted in about 25% higher NOx emissions than B0 at 0 kW and about 45% higher at other loads. This observation is consistent across multiple studies, such as [22,25]. The higher NOx-producing characteristic of biodiesel blends is believed to be largely injection related [14,26]. It can be effectively reduced with the widespread addition of the SCR (selective catalytic reduction) systems. However, studies indicated biodiesel blends may result in faster degradation of the SCR catalyst, likely due to the metal components in biodiesel [27,28].
Figure 3 illustrates BPM emission rates (mg PM/kg fuel consumed) for B0, B50, and B100 over different loads. At 0 and 75 kW loads, emission rates from B50 were the lowest by 6 and 50% compared with B0, with an increase of 50% at the 25 kW load. In contrast, B100 produced much higher emission rates than B0 did. A spike occurring at the 25 kW load was observed in both B50 and B100. This suggests that the use of biodiesel blends may be more beneficial to the environment than using 100% biodiesel for engines built in the early 1990s. This is consistent with Guarieiro et al. (2014) [29], who found that emissions are reduced more from B25 and B50 rather than B100.
Higher PM emissions were observed with biodiesel and blends, which have also been reported by only a few studies, such as [30,31,32]. Variations of diesel engines, biodiesel fuel properties (unsaturation, chain length, glycerin content, etc.), testing conditions and sampling conditions, etc. can all contribute to BPM formation. Due to these large arrays of complexity and uncertainties, inconsistencies exist as to biodiesel’s impact on PM formation [14,15].
With more applications of the diesel particulate filter (DPF), it is expected that the PM emissions from biodiesel and diesel will become of less concern. Better yet, biodiesel blends are believed to improve DPF performance, such as by reducing the frequency of regeneration [15].

3.2. Organic Composition of BPM

The organic composition of particulate matter analyzed included methyl esters, n-alkanes, and PAHs. For most compounds, the highest emissions occurred at 25 kW, which is also in agreement with Figure 3.

3.2.1. n-Alkanes

Figure 4 shows the distribution of n-alkanes in particulate matter from B0, B50, and B100 under different loads. C17-C19 were the highest, followed by C20 and C16, consistent with Liang et al., 2005 [19]. n-Alkanes for B50 were at much lower levels, more than 50% less than B0. Alkanes were also found in BPM from B100, but at much lower quantities and in different patterns. In Figure 4c, the highest alkane concentrations were C20, followed by C17, C18, C16, and C19. These may be from the combustion of methyl ester carbon chains.

3.2.2. PAHs

Particulate phase PAH compounds are shown in Figure 5 for both B0 and B50 respectively under various loads. No PAHs were found in BPM from B100. In addition to acenaphthylene, acenaphthene, fluorene, phenanthrene, and anthracene shown on Figure 5, fluoranthene and pyrene were also identified but in much lower quantities and not at all loads. This is consistent with Popovicheva et al. 2015 [16]. Higher concentrations of PAHs were found at lower loads, such as idling or 25 kW.
The PAH compounds identified were approximately 2% of PM mass for B0, consistent with the 2.5% reported from another study of ours [19], while it yielded only 0.5% of total PM mass for B50. A decrease in PAH formation using biodiesel blends is expected and consistent with literature and is believed to be related to lower toxicity in biodiesel blends.

3.2.3. FAMEs

Figure 6 presents FAMEs found in the BPM of B50 and B100 under various loads. No FAMEs were found from diesel (B0) emissions. Four FAMEs were quantified from BPM, methyl palmitate (C16:0), methyl linoleate (C18:2), methyl oleate (C18:1), and methyl stearate (C18:0). The highest amount of FAME emissions per unit of fuel consumed occurred at 0 kW and decreased with load increase. FAMEs in B100 followed trends similar to B50, with similar concentrations.
This finding is consistent with functional group analysis via FTIR and TG-MS analysis of m/z ratios [17,18]. However, the significant enrichment of C18:2 methyl esters (approximately 71% in BPM as opposed to 52% in biodiesel fuel), together with much lower C18:1, are not well understood. One possibility may be that C18:2 has a lower boiling point (192 °C) than C18:1 (218 °C).
Figure 7 presents the fractions of BPM composition relative to the total mass, and “elemental carbon” here refers to the insoluble part on the filter. The FAME fractions of the BPM were the highest for all loads and ranged from 6 to 11% of the total particulate matter collected. This fraction was approximately 35% of the SOF in B50. This may be an indication that a higher fraction of the biodiesel remains unburnt and may be related to the characteristics of the non-road engine or the BPM sampling method (e.g., dilution), etc. The higher SOF observed from biodiesel blends are likely due to the FAME fractions. More evaporation of FAME fuel is expected, since the boiling points of FAMEs are generally lower than those hydrocarbons with the same carbon chains in the diesel fuel.
The carbon fractions of BPM were further analyzed as shown in Table 1 using NIOSH method 5040. The EC fractions of the particulate matter at B50 are lower than B0 at all loads, while the OC fractions are higher for B50. Higher OC fractions indicate that the use of biodiesel blends tends to increase the SOF (soluble organic fraction) of the particulate matter, which has been reported by many [14,15]. BPM filters used with B50 and B100 were visually much lighter in color than those used for B0, especially at lower loads of 0 and 25kW, which is an indication of less elemental carbon [13]. Similar trends in load variation can be observed for both B50 and B0, in that EC fraction increased with loads, while those of OC decreased. This is consistent with Liu et al., 2005 [24].

4. Discussion

One limitation of this study is that we did not find nitro-PAHs or oxy-PAHs in the BPM of biodiesel blends, which have been reported by some studies [33,34]. This might be due to the lower concentrations of these compounds or the more sophisticated detection analytical methods required, such as higher column temperature (300 °C) and negative CI mode [34]. These PAHs are more toxic, although present in much lower concentrations.

5. Conclusions

Air emissions from a non-road diesel generator were characterized under four loads from idle to 75 kW at 25 kW increments, and with three fuels, petroleum diesel (B0), B50, and 100% biodiesel. Carbon monoxide decreased with biodiesel use (B50 and B100) compared with B0, while carbon dioxide increased. NOx and particulate matter emissions were higher from B50 and B100 than B0. The PAH compounds from B50 are much less than B0, which may be linked to the lower toxicity of biodiesel blends. In the BPM, FAME (the fuel fraction) constituted 6% to 11% of the total mass and was the highest fraction of the SOF. This is an indication that the biodiesel blend might not be well burnt in this diesel engine. This information has not been reported by other studies, which is likely due to the complexity of analysis. The majority of the biodiesel organic emissions comprised of methyl esters, which indicates significant quantities of unburned fuel in the exhaust. Higher soluble organic compositions (OC) were observed in B50 than B0, and conversely with less EC (soot). A decrease in PAHs and the amount of soot can diminish the overall detrimental effects of diesel-powered engines.

Author Contributions

Conceptualization, M.L. and M.C.; methodology, M.L., A.T. and M.C.; experiments and analysis, A.T. and M.C.; writing—original draft preparation, A.T., M.C. and M.L.; writing—review and editing, M.L. and O.A.; project administration, M.L.; funding acquisition, M.L. All authors have read and agreed to the published version of the manuscript.

Funding

Funding from the RET (Research Experiences for Teachers) program of the National Science Foundation (NSF) is acknowledged for providing partial financial support for students. Funding from the NSF PFI program (grant #1919114) and the UC co-op fellowship are also acknowledged for providing student financial support.

Data Availability Statement

Most of the data used in this paper are published in forms of thesis, conference and journal papers. The data presented in this study are available upon request.

Acknowledgments

Dr. M. Eileen Birch’s (NIOSH) assistance in OC/EC analysis is gratefully acknowledged.

Conflicts of Interest

The authors declare no conflict of interest. The funders had no role in the design of the study; in the collection, analyses, or interpretation of data; in the writing of the manuscript; or in the decision to publish the results.

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Figure 1. The schematic diagram of BPM sampling system.
Figure 1. The schematic diagram of BPM sampling system.
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Figure 2. Emissions of carbon monoxide (a), carbon dioxide (b) and nitrogen oxides (c).
Figure 2. Emissions of carbon monoxide (a), carbon dioxide (b) and nitrogen oxides (c).
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Figure 3. BPM emission rates as a function of engine load for B0, B50 and B100.
Figure 3. BPM emission rates as a function of engine load for B0, B50 and B100.
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Figure 4. N-alkane compounds from BPM for B0 (a), B50 (b), and B100 (c) fuels.
Figure 4. N-alkane compounds from BPM for B0 (a), B50 (b), and B100 (c) fuels.
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Figure 5. PAHs identified from BPM for B0 (a) and B50 (b).
Figure 5. PAHs identified from BPM for B0 (a) and B50 (b).
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Figure 6. Methyl esters identified from BPM for B50 (a) and B100 (b) fuels.
Figure 6. Methyl esters identified from BPM for B50 (a) and B100 (b) fuels.
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Figure 7. BPM organic composition by category under different loads at B50.
Figure 7. BPM organic composition by category under different loads at B50.
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Table
Table 1. OC/EC fractions for B0 and B50 under different loads.
Table 1. OC/EC fractions for B0 and B50 under different loads.
B0 B50
Load (kW)ECOCOC/EC RatioECOCOC/EC Ratio
00.250.662.680.180.693.74
250.310.591.930.090.657.09
500.350.421.190.250.622.48
750.530.310.580.370.461.23
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Lu, M.; Tzillah, A.; Chai, M.; Aloraimi, O. Compositional Analysis of Biodiesel Particulate Matter (BPM) from a Non-Road Diesel Generator. Energies 2023, 16, 5010. https://doi.org/10.3390/en16135010

AMA Style

Lu M, Tzillah A, Chai M, Aloraimi O. Compositional Analysis of Biodiesel Particulate Matter (BPM) from a Non-Road Diesel Generator. Energies. 2023; 16(13):5010. https://doi.org/10.3390/en16135010

Chicago/Turabian Style

Lu, Mingming, Aisha Tzillah, Ming Chai, and Omer Aloraimi. 2023. "Compositional Analysis of Biodiesel Particulate Matter (BPM) from a Non-Road Diesel Generator" Energies 16, no. 13: 5010. https://doi.org/10.3390/en16135010

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