Katerina Swanson
Sulfur is a naturally occurring element that is found in many amino acids and proteins essential for life on Earth. It is also present in crude oil and, consequently, in diesel fuel derived from it. Sulfur in diesel fuel has detrimental effects on combustion and emission characteristics, causing air pollution and harmful corrosion in engines. Therefore, it is important to detect and quantify sulfur content in diesel fuel to ensure it complies with regulations and to minimise negative health and environmental impacts. Various test methods exist to measure sulfur content, such as the ASTM method D2622, which uses wavelength dispersive X-ray fluorescence to quantify sulfur concentration. This method is compatible with a wide range of fuel types, including diesel, and offers excellent sensitivity and fast data acquisition.
Characteristics and Values of Detecting Sulfur in Diesel Fuel
| Characteristics | Values |
|---|---|
| Test Method | ASTM D 6428 |
| New Test Method | Performance-based criteria |
| Current Standard for On-Road Diesel in the US | Ultra-low-sulfur diesel fuel |
| Allowable Sulfur Content in the US | Less than 15 ppm |
| Test Method for Sulfur in Petroleum | ASTM D2622 |
| Limit for Sulfur in Diesel in the EU | 10 ppm |
| Limit for Sulfur in Red Diesel Class D | 0.1% (1000 ppm) |
| Countries Using Diesel Fuel with High Sulfur Content | Iraq, Iran, Pakistan, Afghanistan |
| Effects of High Sulfur Content | Damage to engine components, air pollution, harmful corrosion in the engine |
| Solutions to Reduce Sulfur Content | Gasoline-diesel blends, PPCI mode combustion, biodiesel, nano-alumina suspension, bioethanol |
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What You'll Learn
ASTM method D2622
The technique is compatible with a wide range of fuel types, including diesel fuel, jet fuel, kerosene, crude oil, and biodiesel, as well as other distillate oil, naphtha, residual oil, lubricating base oil, hydraulic oil, unleaded gasoline, and gasoline-ethanol blends. The test method is rapid and precise, with a typical analysis time of 1 to 2 minutes per sample.
The ASTM method assumes that the standard and sample matrices are well-matched, and any differences are correctly accounted for to avoid discrepancies that could arise from matrix effects. Instrument calibration for WDXRF instruments is performed using sulfur-containing certified reference materials (CRMs) that cover a range of concentrations and match the real samples' matrix conditions.
The determination of total sulfur content in liquid petroleum and petroleum products can also be achieved using a more powerful instrument, such as the Rigaku Supermini 200, which is a high-performance, high-sensitivity benchtop multielement wavelength dispersive analyzer. This instrument can determine any element from Oxygen to Uranium in solids, liquids, powders, alloys, and thin films.
Overall, ASTM method D2622 is a sensitive, accurate, and fast method for detecting sulfur in diesel fuel and other petroleum products.
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Wavelength dispersive X-ray fluorescence
The WDXRF technique involves the use of X-ray fluorescence to analyze the spectral emission of sulfur in different valence states. This allows for the detection of sulfur in its various inorganic species, such as sulfide, elemental sulfur, thiosulfate, sulfite, and sulfate. The analysis focuses on the spectral lines in the S Kα wavelength range, where Mo Lα (2θ = 111.799°) lines interfere with S Kα (2θ = 110.683°) lines.
One of the key advantages of using WDXRF for measuring sulfur concentrations is its excellent sensitivity. It also offers relatively straightforward sample preparation and fast data acquisition speeds, with samples often being measured in just a few minutes. This makes it a crucial tool for regulatory compliance, as many new requirements mandate very low sulfur concentrations in fuels.
However, one challenge with WDXRF is the effect of the sample matrix on the measured fluorescence. The sample matrix includes all the elements present in the sample, such as C, H, and O, and can impact the accuracy of sulfur detection. To address this, researchers have employed the WD-XRF technique to study the spectral line shifts and matrix effects of different sulfur species, analyzing the interference of other elements on the spectrum of sulfur S Kα lines.
Overall, WDXRF is a valuable and widely used method for detecting sulfur in diesel fuel, offering high sensitivity, rapid results, and compatibility with a range of fuel types.
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High sulfur fuel issues
High sulfur fuel is a problem for modern European engines, which are not designed to run on it. These engines require very low sulfur diesel fuel, typically less than 15 parts per million (PPM). However, some parts of the world still have sulfur levels in excess of 5000 PPM, such as Iraq, Iran, Pakistan, and Afghanistan. High sulfur fuel can cause issues with the engine, as when it gets into the engine oil, it breaks down the oil's lubricating properties, potentially leading to engine damage. This can occur during the power stroke as the fuel gets blown past the piston rings. The issue is exacerbated during the Diesel Particulate Filter (DPF) regeneration cycle, when the fuelling is modified to increase the exhaust temperature.
High levels of sulfur in diesel fuel can also lead to high levels of particulate matter (PM) in the exhaust emissions, as well as the production of SOx and H2S. This can contribute to air pollution and the formation of acidic aerosols that cause acid rain, snow, and fog. Additionally, around 95% of the sulfur combusted in fuel is emitted as sulfur dioxide (SO2), a toxic gas linked to serious human health issues. This includes increased asthma, heart disease, and respiratory disease.
The process of purifying diesel fuel from sulfur requires new refineries and the disposal of the extracted sulfur, which is not feasible in some countries. However, there have been studies on reducing the negative impacts of high sulfur fuel. For example, the addition of biodiesel fuel to high-sulfur diesel has been found to reduce pollutant emissions, especially with increasing methyl ester portions in the fuel blend. Additionally, the use of low SAPS oils, which contain reduced quantities of Sulphated Ash, Phosphorus, and Sulphur, can help prevent the blocking of the DPF.
The presence of sulfur in diesel fuel can also impact the monetary value of the product. The European Union has set a limit of 10 PPM of sulfur for all diesel and gasoline, while the US has adopted ultra-low-sulfur diesel fuel as the standard for on-road diesel, allowing less than 15 PPM.
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Ultra-low-sulfur diesel
The move towards ULSD allows for the application of advanced emissions control technologies that substantially lower the harmful emissions from diesel combustion. Engine manufacturers and regulatory bodies have found that the use of emissions control devices in conjunction with ULSD can reduce the exhaust output of ozone precursors and particulate matter to near-zero levels.
There are varying standards for ULSD globally. In the European Union, the "Euro IV" standard has applied since 2005, which specifies a maximum of 50 parts per million (ppm) of sulfur in diesel fuel for most highway vehicles. ULSD, with a maximum of 10 ppm of sulfur, has been widely available since 2008. In 2009, the Euro V fuel standard came into effect, further reducing the maximum sulfur content to 10 ppm for most diesel fuel applications.
In the United States, ULSD with a maximum sulfur content of 15 ppm has been the standard for on-road diesel fuel since 2006, except for rural Alaska, which transitioned in 2010. All diesel fuel sold in the U.S. must be ULSD, and pumps dispensing ULSD must be labeled as such, except in California.
In India, Bharat Stage VI with an ultra-low sulfur content of less than 10 ppm became the standard across the country from April 2020.
Various test methods are available to detect and quantify the sulfur content in diesel fuel, such as the ASTM method D2622, which uses wavelength dispersive X-ray fluorescence (WDXRF) to measure sulfur concentrations.
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Sulfur's impact on engine oil
Sulphur is naturally occurring in mineral oils and an additive in synthetic oils. It is a protective additive that acts as a metal deactivator, reducing the catalytic effect of metals on the oxidation rate. It is also an anti-wear component and helps dissolve other additives.
However, sulphur is one of the contaminants that kill catalytic converters. When high-sulphur fuel is used, sulphuric acids are the most significant corrosive acids formed. These acids cause corrosive wear on the metal surfaces of an engine. Sulphur also negatively impacts combustion and emission characteristics, leading to high levels of PM, SOx, and H2S.
Regulations to reduce vehicle emissions have dramatically reduced the allowable sulphur content in diesel fuel. Today, sulphur content in diesel fuel in the United States and Mexico is 97% lower than in the 20th century. This type of fuel is referred to as ultra-low-sulphur diesel (ULSD).
To prevent organic acid corrosion with ULSD fuel, engine oil formulations require a complex mix of detergent, antioxidant, and corrosion inhibitor additives.
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Frequently asked questions
Sulfur in diesel fuel creates sulfuric acid, causing corrosive wear on the metal surfaces of an engine. It also forms particulates that are a primary contributor to air pollution.
The standard for sulfur content in diesel fuel varies by region. In the US, ultra-low-sulfur diesel fuel is the standard for on-road diesel, with a maximum sulfur content of 15 ppm. In the European Union, the limit is 10 ppm for all diesel and gasoline. Other regions have even lower limits of 0.1% m/m.
One standard test method for detecting and quantifying sulfur content in diesel fuel is ASTM D2622, which uses wavelength dispersive X-ray fluorescence (WDXRF) to measure sulfur concentration. Another test method is ASTM D 6428, although this was originally developed for aromatic hydrocarbons rather than petroleum products.
The level of sulfur in diesel fuel can be reduced by adding gasoline to the diesel and manipulating the fuel injection timings. This results in better and cleaner combustion. Additionally, using ultra-low-sulfur diesel (USLD) or ultra-low sulfur diesel (ULSD) can help minimize the need for detergent additives and reduce sulfuric acid concentrations in exhaust emissions.
