The petrochemical industry performs many tests for refined products. Refineries, Inspection and Chemical labs across the world use ASTM, ISO, IP, and other accepted chemical industry standards and protocols. Materials tested include the entire complex range of hydrocarbon based chemicals derived from petroleum. This also applies to primary petrochemicals including olefins, aromatics, and synthesis gas. Petrochemical testing can extend to trace and ultra-trace level analysis. Chemical testing expertise includes purity & component, trace composition, trace contamination, quality control, troubleshooting, and other chemical analysis expertise. ASTM chemical testing methods are utilized by laboratories for chemical analysis of petrochemicals, compounds, materials, petroleum, fuels, consumer products, and other chemical substances. 

Oil refinery at night.
Oil pumps.

ASTM chemical test methods are industry accepted standards for quality control and reliability. Testing measures require trace analysis to ppm, ppb, and ppt levels. Petrochemicals and chemicals are tested for quality control, purity, contamination, research and development, troubleshooting, environmental evaluation, regulatory compliance, and more. No matter what your combustion applications require EST Analytical has a solution for you. Innovative solutions for liquids, solids, and LPG’s are provided in either our horizontal system the Nexis or vertical system the 7000. EST provides full service, parts and technical support to keep your labs running seamlessly.

Application Types

Total Nitrogen Analysis

Total Nitrogen (TN) stands for the sum parameter of all organic and inorganic nitrogen compounds. Trace levels (0.02 – 10.000 mg/kg or ppm by weight) of Total Nitrogen are measured with an elemental combustion analyzer according to Chemiluminescence detection technique. Total Nitrogen in fuels (NO2) pollutes the environment. It is corrosive to steel and poisons catalysts. Nitrogen compounds are more thermally stable compared to sulfur compounds and is often concentrated in heavier petroleum fractions and residues. Examples of Organic Nitrogen compounds that contribute to the Total Nitrogen number in petroleum products are Pyridines, Quinolines and Carbazoles. Common ASTM methods for nitrogen testing include: ASTM D4629, ASTM D5762, ASTM D7184, and D6069. The NEXIS TN total nitrogen analyzer provides a reliable and robust solution for labs.

Oil refinery and clouds in sky.

Whitepapers

Vacuum Gas Oils (VGOs) are the heavy oils left after petroleum distillation. VGOs have a viscous matrix and high boiling points. The EST Analytical TN 7000 has an injection port designed to maintain the injection port temperature at 500°C, while the autosampler tray can be fitted with a heater. These features aid in making the TN 7000 ideal for the examination of Total Nitrogen in VGO samples.

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Crude oil is composed mainly of hydrocarbons mixed with a variation of nitrogen, sulfur and oxygen. The differences in the nitrogen, sulfur, and oxygen content can be attributed to where the crude oil originates. After drilling, crude oil is usually refined in order to create fuel, lubricants, etc. Due to the use of processing catalysts in the refining method, determining the nitrogen and sulfur content is very important. Trace amounts of sulfur and nitrogen can be very detrimental. Thus, determining the nitrogen and sulfur content is very important. This application will examine total sulfur and nitrogen in light hydrocarbon samples using the NEXIS combustion elemental analyzer, complete with a novel multilayer combustion tube.

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EST Analytical has developed a new signal processing technique to achieve the lowest detection levels for trace level total sulfur and nitrogen for the NEXIS VP model Combustion analyzer. The NEXIS trace level sulfur, nitrogen and chlorine analyzer models equipped with the AS120 liquid/solids autosampler enables laboratories to perform a multiple point calibration line using ONE-Cal™ Technology and the NEXIS LINK software platform including Digital Signal Processing (DSP) Technology™.

This application note shows the analytical data and achieved LOD’s for both nitrogen and sulfur with the NEXIS VP model based on ISO ISO11843-2 methodology and the use of the NEN 7777 method which is incorporated in the NEXIS LINK operating software.

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Nitrogen compounds can have detrimental effects on many environmental and industrial processes and are undesirable in finished products. This support the need and importance to monitor low level nitrogen concentration of various type of automotive fuels and related products. This Application Note shows the of the NEXIS VP model Total Nitrogen Analyzer for a set of gasoline and diesel fuel samples based on a 21-days trial to determine the precision of the nitrogen data in compliance to ASTM D4629 and DIN 51444 methods.

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Labs around the globe share a common need to enhance lab productivty and stability when analyzing Total Sulfur, Nitrgen and Chlorine. Today, that process consumes too much time and money. When done improperly it can also contribute to poor data outcomes requiring labs to repeat calibrations and delay much needed sample analysis.

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ASTM D5762 covers the determination of Total Nitrogen in liquid petroleum products and lubricants in concentrations ranging from about 40 to 10,000 mg/ kg.

Nitrogen compounds can have detrimental effects on many environmental and industrial processes and are undesirable in finished products. Nitrogen containing hydrocarbons seem to be the hardest to hydrotreat, meaning that the nitrogen content in the product of the hydrotreater is a measure of the effectiveness of the hydrotreating process.

This supports the need and importance to monitor trace level nitrogen concentration of various type of automotive fuels and related products. This Application Note shows the Total Nitrogen analysis performance of a set of liquid hydrocarbon samples, by the EST NEXIS model Total Nitrogen analyzer.

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ASTM D4629 covers the determination of Total Nitrogen in concentrations ranging from about 0.3 to 100 mg/kg in liquid petroleum products having a boiling point range of 50˚C to 400˚C and viscosities between 0.2 and 10 mm²/s at ambient temperature. The ASTM D4629 standard is the preferred method in many countries to detect
and quantify total bounded nitrogen containing compounds in the various type of automotive fuels such as blended gasolines, diesel and synthetic oils.

Nitrogen compounds can have detrimental effects on many environmental and industrial processes and are undesirable in finished products. This supports the need and importance to monitor trace level nitrogen concentration of various type of automotive fuels and related products. This application note shows the total bounded nitrogen analysis performance of a set of liquid hydrocarbon samples, by the EST NEXIS Total Nitrogen analyzer.

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The future requirements of Total Sulfur/Nitrogen analysis in light liquid hydrocarbons such like petrochemical base, intermediate and final products are heading towards very low concentration levels (ppb). This application note shows the precision, Level of Detection (LOD) and repeatability performance when a simultaneous analysis of Total Nitrogen and Sulfur is conducted using the NEXIS Combustion analyzer equiped with both ONE-Cal™ functionality and Digital Signal Prcoessing Technology (DSP). DSP Technology will enhance the Sulfur/Nitrogen detector performance resulting in a level of high sensitivity and repeatability.

This note shows the raw analytical calibration data and achieved LOD’s for both Nitrogen and Sulfur using the NEXIS model equipped with the AS120 liquids autosampler in the range of 0 – 1000 ppb.

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ASTM D5762 is an established method for the determination of nitrogen in lubricating oils by oxidative boat inlet chemiluminescence technique. The application is of significant importance because nitrogen components can contaminate refinery catalysts. The determination of nitrogen concentration in lubricant oils is a measure of the total nitrogen in various additives. This application notes describes the principle of operation and obtained analysis results using the NEXIS TN analyzer model, which benefits the customer from ease-of-use, precise total nitrogen data en fast analysis times.

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It is very challenging to analytically and precisely quantify Total Nitrogen concentrations less than 1 ppm in hydrocarbons such as liquid aromatics to be used for synthesis or to be used for various plastic polymerization processes. In order to analyze this kind of Ultra Trace level samples on day-to-day routine lab bases; repeatability with high accuracy and ease-of-use and excellent robust performance is highly required. EST has developed and validated the Ultra Trace Total Nitrogen ranges for the NEXIS and NEXIS VP model analyzers. Concentrations of below 1ppm defined as Ultra Trace Nitrogen are no longer a challenge.

The developed functionalities ONE-Cal™ and DSP Technology™ are made available for everyone and this data demonstrates high sensitivities, repeatabilities and linearities of the Ultra Trace Levels in quantifying Total Nitrogen using the EST NEXIS VP model. The use of the DSP Technology™ which improves the signal to noise ratio on both sides of the equation has been applied to the NEXIS and NEXIS VP. A comparison is made between the DSP function running disabled and enabled and is carried out for specifically in the Ultra Trace regime of the calibration region. The data gained by this comparison can be obtained in this Application Note.

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The oxidative combustion analysis of a wide range of petroleum samples which may contain high sulfur and/or nitrogen content may result into potential carry-over effect issues that can result in downtime for this analysis. The EST NEXIS VP model with AS120 liquid autosampler uses a direct injection technique combined with a high efficiency combustion tube design to avoid the risk of incomplete combustion and therefore demonstrates a very low carry-over effect. This application note describes the practical lab study for the “carry-over effect” and the degree to which the NEXIS VP TN/TS elemental combustion analyzer manages1) the “carry-over” effects which is based on a reference definition. Extreme high sulfur/nitrogen concentrations of 10,000 ppm as well as middle high ppm concentrations 100 ppm of nitrogen and sulfur samples were analyzed multiple times and multiple sets followed by a set of blank solvent injections to determine the “carry-over” effects.

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Quantifying accurately high concentrations of Total Nitrogen in liquid hydrocarbons and solid samples with a Combustion analyzer is dependent on the controlled combustion process and the linearity of the Chemiluminescence detector (CLD). The NEXIS and NEXIS VP models Total Nitrogen analyzer has applications in a wide range of petroleum products including lubricants, resins and a variety of polymer sample types. Normally high range calibration lines show a second order line, which can have a negative impact on the accuracy of the obtained nitrogen test data. This Application Note shows the performance of the NEXIS product at a wide linear working range, without the need to change from typical PMT settings of the CLD detector or the need to perform separate calibration lines.

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Total Sulfur Analysis

Exhaust from a car.

Total Sulfur (TS) stands for the sum parameter of all organic and inorganic sulfur compounds. Trace levels (0.02 – 10.000 mg/kg or ppm by weight) of Total Sulfur are measured with an elemental combustion analyzer according to UV-Fluorescence detection technique or Microcoulometric detection technique. Common ASTM methods for sulfur testing include: ASTM D5453-19a, ASTM D6667, and ASTM D7183. The Nexis TS Total Sulfur analyzer provides a reliable and robust solution for labs.

Environmental regulations like the TIER III and EURO VI wield a maximum of 10 mg/kg of Total Sulfur or ppm by weight in diesel oils. The maximum amount of 10 ppm is also included in the Chinese norms GB 19147-2013 for Diesel fuels and GB 17930-2013 for Gasoline, deriving from the CHINA 5 environmental program.

ASTM Method D5453–19a includes an Appendix (A1) which describes the requirement to compensate for the presence of any nitrogen compound interference when analyzing Trace Level Total Sulfur content in naphtha’s, distillates, engine oils, ethanol, Fatty Acid Methyl Esters (FAMEs) and engine fuels.

Some analyzers today use a back-order calculation to manage nitrogen interference. However, it is limited in that it’s mathematical only and does not change the composition of the NO matrix. It also requires the added cost of a nitrogen analyzer. Others change the NO prior to UV detection. This can be very effective but may reduce the lifespan of the UV detector reaction chamber. The Nexis TRINITY solution changes the NO prior to UV detection. Its adjustable capability does not impact the lifespan of the UV detection chamber; therefore, making it the ideal solution for trace level sulfur detection.

Oil refinery structures.

Whitepapers

Crude oil is composed mainly of hydrocarbons mixed with a variation of nitrogen, sulfur and oxygen. The differences in the nitrogen, sulfur, and oxygen content can be attributed to where the crude oil originates. After drilling, crude oil is usually refined in order to create fuel, lubricants, etc. Due to the use of processing catalysts in the refining method, determining the nitrogen and sulfur content is very important. Trace amounts of sulfur and nitrogen can be very detrimental. Thus, determining the nitrogen and sulfur content is very important. This application will examine total sulfur and nitrogen in light hydrocarbon samples using the NEXIS combustion elemental analyzer, complete with a novel multilayer combustion tube.

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ASTM Method D5453 is commonly used to determine Total Sulfur in liquid hydrocarbons. The boiling range of these hydrocarbons can vary from 25 to 400ºC. This method calls for the sample to be directly injected or placed in a sample boat and then inserted into a high temperature tube for combustion where the sample is oxidized into sulfur dioxide (SO2). The sample is exposed to ultraviolet light and detected by a photomultiplier. This application note will examine the Total Sulfur content of diesel fuel samples using the NEXIS Total Nitrogen/Total Sulfur combustion analyzer.

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ASTM Method D5453-19a describes the combustion and Ultra Violet Fluorescence (UV-F) detection of Sulfur in light hydrocarbons, engine fuels and oils. However, even an optimized detector may identify nitrogen oxide as Sulfur dioxide, as they both emit at the same wavelength. This problem can result in false positives or biased total sulfur data. EST Analytical has developed an integrated tunable Nitrogen Oxide interference elimination module, called the TRINITYTM Module. This new module ensures there is no interference when analyzing high nitrogen containing samples thus delivering accurate total Sulfur data.

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ASTM D5453 covers the determination of Total Sulfur in concentrations ranging from about 1 to 8000 mg/kg in a wide range of liquid hydrocarbons and automotive fuels having a boiling point range of 25˚C to 400˚C and viscosities between 0.2 and 20 Cst (mm²/s) at ambient temperature.

Sulfur compounds can have detrimental effects on many environmental and industrial processes and are undesirable in finished products. This supports the need and importance to monitor trace level sulfur concentration of various type of automotive fuels and related products. This Application Note shows the analysis performance of a set of automotive fuel samples. The system design and methodology of the EST NEXIS Total Sulfur analyzer is thoroughly tested for response linearity and repeatability, to validate its performance according to ASTM D5453.

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EST Analytical has developed a new signal processing technique to achieve the lowest detection levels for trace level total sulfur and nitrogen for the NEXIS VP model Combustion analyzer. The NEXIS trace level sulfur, nitrogen and chlorine analyzer models equipped with the AS120 liquid/solids autosampler enables laboratories to perform a multiple point calibration line using ONE-Cal™ Technology and the NEXIS LINK software platform including Digital Signal Processing (DSP) Technology™.

This application note shows the analytical data and achieved LOD’s for both nitrogen and sulfur with the NEXIS VP model based on ISO ISO11843-2 methodology and the use of the NEN 7777 method which is incorporated in the NEXIS LINK operating software.

Learn More >>

Labs around the globe share a common need to enhance lab productivity and stability when analyzing Total Sulfur, Nitrogen and Chlorine. Today, that process consumes too much time and money. When done improperly it can also contribute to poor data outcomes requiring labs to repeat calibrations and delay much needed sample analysis.

Learn More >>

ASTM D5453 covers the determination of Total Sulfur in concentrations ranging from about 1 to 8,000 mg/kg in a wide range of liquid hydrocarbons and automotive fuels having a boiling point range of 25˚C to 400˚C and viscosities between 0.2 and 20 Cst (mm²/s) at ambient temperature.

Sulfur compounds can have detrimental effects on many environmental and industrial processes and are undesirable in finished products. This supports the need and importance to monitor trace level sulfur concentration of various type of automotive fuels and related products. This application note shows the analysis performance of a set of automotive fuel samples. The system design and methodology of the EST NEXIS Total Sulfur analyzer is thoroughly tested for response linearity and repeatability, to validate its performance according to ASTM D5453.

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The EST NEXIS GM model, Gas & LPG Sample introduction module, is able to accurately sample and automatically introduce Gases and LPG samples into the EST NEXIS model Total Sulfur Analyzer. This feature results into a fully automatic calibration and sample analysis for trace level Total Sulfur content with the EST NEXIS series TS analyzers. Liquefied Petroleum Gas (LPG) is a group of hydrocarbon gases easily liquefied at moderate pressures which typically comprise C1 up to C10 hydrocarbons and S hetero compounds. The most common forms of LPG are methane (CH4),

Ethane (C2H6), propane (C3H8), propylene (C3H6), butanes (C4H12) and butylenes (C4H8). The most common S compounds found in LPG are sulfides, thiophenes and mercaptans.

LPG originates from two main sources: Associated gases in crude oils and gases produced in the refining processes. Because of its origin the composition of LPG varies in a wide range of components and concentrations. When processed industrial and domestic use as a fuel, hydrocarbons >C3 are removed since they are very valuable in petrochemical processes and gasoline blending operations. This type of fuel is a colorless and odorless mixture to which a certain amount of S compounds odorants is added to facilitate its detection. The determination of the total sulfur (TS) content in LPG streams is important to prevent sulfur related pipelines and equipment corrosion; to improve the quality of final products and to reduce pollutant emissions into the atmosphere.

LPG and other light hydrocarbons also find use as feedstocks for a variety of new refining catalytic technologies. The need for low sulfur measurements in this part of the industry is of growing importance since sulfur compounds poison the catalysts and negatively impact the economics of the processes. Furthermore, LPG is increasingly used as an automotive fuel and must therefore comply with stringent legislations concerning their Total Sulfur content.The Total Sulfur analysis of LPG by UV-Fluorescence detection is governed by ASTM D6667 and is applicable to samples containing sulfur in the range of 1.0 to 100 mg/kg. This application note describes a direct sampling and injection technique, which is fully compliant with ASTM D6667, for measuring low level sulfur in LPG using the EST NEXIS model Total Sulfur Analyzer in conjunction with the EST NEXIS GM model, Gas & LPG Sample introduction module.

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The future requirements of Total Sulfur/Nitrogen analysis in light liquid hydrocarbons such like petrochemical base, intermediate and final products are heading towards very low concentration levels (ppb). This application note shows the precision, Level of Detection (LOD) and repeatability performance when a simultaneous analysis of Total Nitrogen and Sulfur is conducted using the NEXIS Combustion analyzer equiped with both ONE-Cal™ functionality and Digital Signal Prcoessing Technology (DSP). DSP Technology will enhance the Sulfur/Nitrogen detector performance resulting in a level of high sensitivity and repeatability.

This note shows the raw analytical calibration data and achieved LOD’s for both Nitrogen and Sulfur using the NEXIS model equipped with the AS120 liquids autosampler in the range of 0 – 1000 ppb.

Learn More >>

The oxidative combustion analysis of a wide range of petroleum samples which may contain high sulfur and/or nitrogen content may result into potential carry-over effect issues that can result in downtime for this analysis. The EST NEXIS VP model with AS120 liquid autosampler uses a direct injection technique combined with a high efficiency combustion tube design to avoid the risk of incomplete combustion and therefore demonstrates a very low carry-over effect. This application note describes the practical lab study for the “carry-over effect” and the degree to which the NEXIS VP TN/TS elemental combustion analyzer manages1) the “carry-over” effects which is based on a reference definition. Extreme high sulfur/nitrogen concentrations of 10,000 ppm as well as middle high ppm concentrations 100 ppm of nitrogen and sulfur samples were analyzed multiple times and multiple sets followed by a set of blank solvent injections to determine the “carry-over” effects.

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Total Chlorine Analysis

Total Chloride, Total Chlorine or Total Halogens, stand for the sum parameter of organic as well as inorganic Fluorine (F), Chlorine, (Cl), Bromine (Br) and Iodine (I). Trace levels of Total Chloride are measured with an elemental combustion analyzer according to Microcoulometric detection technique / Microcoulometry. Organic chlorines do not occur naturally in crude oil. When present, they result from contamination in some manner, such as disposal of chlorinated solvent used in many dewaxing pipeline or other equipment operations. Organic Chlorine species are potentially damaging to refinery processes. Hydrochloric acid can be produced in hydrotreating or reforming reactors and the acid accumulates in condensing regions of the refinery. Unexpected concentrations of organic chlorides cannot be effectively neutralized and damage can result. Organic chlorides are not known to be naturally present in crude oils and usually result from cleaning operations at producing sites, pipelines, or tanks. It is important for the oil industry to have common methods available for the determination of organic chlorides in crude oil, particularly when transfer of custody is involved. Common ASTM methods for chloride testing include: ASTM D5194, ASTM D4929, D5808, D6721, and D7457. The Nexis TX total chloride analyzer provides a reliable and robust solution for labs.

 

Oil refinery at dusk.

Whitepapers

The presence of chlorine in crude oil can hydrolyze during the refinery process to form hydrochloric acid which causes corrosion. Corrosion at petroleum refineries is a critical problem which exists at many places around the globe and has a huge cost impact in terms of maintenance.
Therefore, an effective chloride monitoring solution should be implemented and many refineries have a periodic testing of inorganic chlorides in place. A well-known, reliable and sensitive test method for the chlorine analysis in crude and fuel oil products is oxidative micro coulometric technique which has been applicable at the EST Total Chlorine analyzer, model NEXIS TX.

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Waste generated by agro-food industries can result in environmental contamination and impact the costs involved in controlling and reducing this
harmful environmental effect through stringent legislations.
The generation of bio-energy and availability of renewable fuels as a biodegradable source will help to lighten the environmental pollution grade and have already been introduced and implemented in many countries. Exhaust emissions of sulfur oxides, nitrogen oxides, carbon monoxide and unburned hydrocarbons are significantly lower with biodiesel usage in comparison to mineral diesel, which can dramatically reduce the impact on the environmental. The presence of chlorinated compounds in these types of products can negatively affect the lifespan and effectiveness of catalyst material used in the process of biodiesel production. The regular chlorine concentrations of the refined biodiesel and animal fat raw materials are at trace ppm level, which are determined quantitatively by oxidative combustion micro-coulometric detection technique. This Application Note describes the principle, procedure and performance data of a Total Chlorine analysis in original/raw animal fat samples using the EST NEXIS TX Analyzer in accordance with ASTM D4929

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