2018 Posters

The following posters will be presented in the Exhibit Hall at the 2018 Gulf Coast Conference.

Abstract # 102 - Poster - 10/17/2018 - 10:00 AM - South Lobby

EDXRF Technology’s Applications to Measure the Sulfur Content in Ultra-Low Sulfur Fuels and to Measure Organometallic Additives in Lubrication Oils and Motor Gasoline.

Raj Shah - Koehler Instrument Company, Inc.
Arthur Rozario - Koehler Instrument Company, Inc.
Scott Fess - Applied Rigaku Technologies, Inc.

The Energy Dispersive X-ray Fluorescence Spectrometry (EDXRF) is a fast, simple, and non-destructive analysis technique for the measurement of liquids, powders, and solids. It is widely applied throughout the petroleum industry: upstream at the well site, mid-stream at pipelines, storage facilities and blending operations, and down-stream at the refinery.  Recently, with the Environmental Protection Agency (EPA) mandating new regulations on the composition of fuel, the maximum allowable sulfur content has been scaled down to 10 parts per million (ppm). Therefore, the EDXRF is an ideal analytical tool for refiners - with good lab practices- to accurately determine the sulfur content in fuel samples, conforming to not only ASTM D7220, but also meeting the testing requirements for the EPA Tier 3 program for ultra-low sulfur fuels such as gasoline and diesel. Furthermore, the EDXRF can be used to determine concentration of some elements such as manganese, lead, zinc, phosphorous, and calcium. The determination of manganese and lead content gives an indication of the anti-knock agent added to motor gasoline and Avgas to improve octane rating.  Whilst the determination of zinc, phosphorous, calcium, and Sulfur give an indication of the antioxidant, and antiwear agents in lubricating oils. The versatile application of the EDXRF allows end-users to effectively ascertain correct results for this desired use, and conform to international testing standards.

Abstract # 103 - Poster - 10/17/2018 - 10:30 AM - South Lobby

Innovative Instrumentation Design for Measuring Multiple Fuel Properties in Diesel Fuel

Raj Shah - Koehler Instrument Company, Inc.
Arthur Rozario - Koehler Instrument Company, Inc.
Wayne Smith - Real-Time Analyzers

The efficiency, economy, and reliability of diesel engines has made it popular for use in transportation, manufacturing, power generation, construction, and farming.  In 2004, 60 percent (%) of trucks in the United States was recorded to consume diesel fuel. In fact, the sales of diesel fuel are an indicator of economic strength, as diesel engines are commonly used to move goods from manufacturer to consumer. It is advantageous to the end-user or consumer to have a reliable and effective way to quickly determine properties of a fuel. However, determining the properties of fuel can be a time-consuming process. Therefore, the Portable Fuel Property Analyzer (PFPA) is an innovative technique developed for fuel quality assessment for in-field analysis of diesel fuel that can be compared to the governing ASTM requirements.   The PFPA combines Near Infrared Spectroscopy with Advanced Chemometric Analysis to determine key fuel properties that must meet specification standards.  The PFPA correlates a database of NIR spectra to fuel properties that were determine with traditional ASTM methods using partial least squares (PLS). The PLS models were then compared to a validation set of fuel samples.  The predicted values of PFPA exhibit comparable accuracy to ASTM methods and the repeatability values often-exceeding ASTM repeatability values. In contrast to standard ASTM test methods, which require a specific instrument for each property and a large volume of fuel sample, the PFPA can determine multiple fuel properties of diesel fuel in 10 seconds using only 2ml of sample. This allows end-users to test diesel fuel rapidly, and to quickly determine if it meets fuel specification requirements.

Abstract # 106 - Poster - 10/17/2018 - 1:00 PM - South Lobby

Recent Advances in a Unique Laboratory Technique SRV® to Study and Help Solve a Wide Range of Tribological Real-life Problems

Raj Shah - Koehler Instrument Company

The SRVÒ test system- where SRV stands for the German acronym for oscillation, friction and wear – provides diverse model test environment for evaluating the friction and wear properties of lubricants, greases and materials.

Due to its versatile application this test system is appealing to be adopted by the industry to test their components in setups with high practical relevance and in conjunction with lubricants, materials and layers. In this study, a reciprocal model test has been applied that reproduces the real load situation of the contact of piston ring and cylinder linear at Fired Top Dead Center (FTDC) of internal combustion engines. Friction, wear, and load carrying capacity (LCC) were analyzed as a function of temperature, oil supply rate, and normal force for grey cast iron and spray coated cylinder liners, different piston ring coatings and engine oils. The test results show a significant dependency of the LCC on changing temperature and oil supply rate corresponding to different cylindrical pressures. Furthermore, the SRVÒtechnology is in compliance with 19 ISO, DIN, and ASTM testing standards developed by the SRVÒstandardization work group. As the established industry standard for friction and wear testing, the SRVÒprovides high precision results that help solve a wide range of tribological real-life problems.

Abstract # 107 - Poster - 10/17/2018 - 11:30 AM - South Lobby

Evaluation of Degradation Degree of Lubricating Oil Using Thermal Desorption and Pyrolysis Combined with DART-MS and Kendrick Mass Defect Analysis

CHIKAKO TAKEI - BioChromato, Inc.

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Lubricating oil is composed of base oil and additives. In order to analyze the base oils and additives of lubricating oils, complicated pretreatment which takes a lot of time and effort were required, generally. However for R&D, QC and market research, it is important to obtain the information on base oils and additives. Recently, thermal desorption and pyrolysis/direct analysis in real time (TDP/DART)-MS and Kendrick Mass Defect (KMD) analysis is using for polymer analysis, respectively. The purpose of this work to Analysis directly and evaluate the degradation degree of lubricating oils. In the thermal desorption region, a phenol type antioxidant, an amine type antioxidant, a salicylic acid type detergent dispersant were detected and determined from all samples. No significant difference in the amount ratio of additive components at 0 km and 1000 km running, but at 5000 km, salicylic acid type detergent and phenolic antioxidant was remarkably decreased. Therefore, TDP/DART-MS enables evaluation of degradation degree of lubricating oils using the additive intensity as a marker. In the pyrolysis region, using KMD analysis, the glycol compounds were detected by automobile running, clearly. And it increased with increasing in mileage. It was assumed that the glycol compounds were one of degradation compounds of lubricating oils. Therefore, KMD analysis was valuable way to search the differences between complex mass spectra. In summary, a combination of TDP/DART-MS and KMD analysis enables analysis both additives and base oil without any pretreatment. Therefore, the combination can contribute to elucidate of the degradation mechanism, failure analysis, R&D, and quality control in the field of automobiles.

Abstract # 119 - Poster - 10/17/2018 - 11:30 AM - South Lobby

Application of ASTM Test Methods to Analyze the Oxidation Properties of Automotive Gasoline in Various Test Conditions

Dr Raj Shah - Koehler Instrument Company
Tahseen Tabassum - Koehler Instrument Company

Determination of oxidation properties of petroleum products is important to determine their reactivity in the presence of air, moisture and organic compounds. Petroleum products are unstable as they form gum upon aging in the presence of air which is directly related to oxidation of gasoline. As the oxidation occurs in the system, the molecules of oxygen decrease resulting in the pressure drop in the system. Additionally, the presence of sulfur and other organic molecules can accelerate the oxidation in gasoline. The current method ASTM D525 Standard test method for oxidation stability of gasoline (Induction period method) covers the determination of the stability of gasoline under accelerated oxidation conditions and ASTM D130 Standard Test Method for Corrosiveness to Copper from Petroleum Products by Copper Strip Test was applied to determine the oxidation condition of gasoline in the presence of sulfur contamination. In this study ASTM D130 and D525 was performed to determine the oxidation properties of gasoline sample in the presence of air, moisture and additives. Scanning Electron Microscopy (SEM) imaging techniques were used to compare the rust formed in the Cu-strips during the oxidation process.

Abstract # 120 - Poster - 10/17/2018 - 2:30 PM - South Lobby

Ongoing Developments of ILSAC GF-6 Engine Oils Standards

Raj Shah - Koehler Instrument Company, Inc.
Christin Abraham - Stony Brook University

Approximately 30 percent of the total United States GHG emissions are generated by the transportation sector. Recent updates to the Corporate Average Fuel Economy (CAFÉ) legislation require passenger cars and light trucks to attain an average fuel economy of 54.5 MPG by 2025. Upcoming ILSAC GF-6 certified engine oils will need to meet CAFÉ requirements. In this poster, the current state of ILSAC GF-6 will be discussed, including the need for a new standard, reasons for the repeated delays, improvements made over the preceding GF-5, and how close we are to first authorized use.

Abstract # 122 - Poster - 10/17/2018 - 3:00 PM - South Lobby

Assessment of Biodiesel Quality Test Methods Used in Middle Distillate Fuels

Raj Shah - Koehler Instrument Company, Inc
Aristidis Mihalos - Stony Brook University

In recent years, biodiesel has proven to be a good alternative fuel option on the basis of its carbon neutral footprint, sustainability, and economic viability. In the early 2000s, biodiesel regulation was insufficient and not properly integrated in the industry. Biodiesel from this time period often lead to various issues including engine clogging problems. Thus, producing high quality biodiesel is paramount to the success of a petroleum-based fuel alternative. Seeing the need in the marketplace, the National Biodiesel Board collaborated with the Vehicle Technologies Office to improve the specifications for B100 biodiesel blend stocks that are to be mixed with middle distillate fuels in ASTM D6751: Standard Specification for Biodiesel Fuel (B100) Blend Stock for Distillate Fuels. This paper serves to introduce the different biodiesel testing methods in D6751 and to elucidate the significance and limitations of each test. Additionally, the paper discusses other biodiesel test methods used in Europe and elsewhere that may be beneficial for ASTM D6751 to consider in the future.

Abstract # 126 - Poster - 10/17/2018 - 10:00 AM - South Lobby

Analysis of Industrial Polymer Application Defects by GC×GC

Christian Wold - SABIC
Eric Brander - SABIC
Jan Willem Heuseveldt - SABIC
Jos Dekkers - SABIC

This work outlines the use of GC×GC in a practical industrial setting for polymer application development. During the development cycle of new products, some questions may arise during prototyping and upscaling that require detailed chemical characterization.   The GC×GC technique is very powerful, particularly in combination with a variety of sample introduction techniques depending on the nature of the material to be examined. Equally important, the technique offers an exceptional way to visualize differences in samples, that may be reported and explained quite easily to non-chemists.   This work demonstrates the applicability of GC×GC to understand the performance of polymers in applications by comparing and processing complex 2D chromatograms. For example in a household lighting application, visual inspection of the GC×GC 2D plots and analysis of MS data were used to establish the chemical differences between four subassembly parts. Based on the GC×GC data it was possible to propose an improvement in the process of product development. In another application, polymer sheets exhibiting differences in color and light transmittance were studied by GC×GC. The obtained 2D contour plots were compared to highlight which components were likely to be responsible for the color change and transmittance alteration.   Finally, the benefits and challenges of GC×GC for polymer analysis were evaluated and will be addressed.

Abstract # 128 - Poster - 10/17/2018 - 3:30 PM - South Lobby

The effect of intermolecular forces and entropy on viscosity, vapor pressure and evaporation in hydrocarbon oils

Tom Karis - TEK Data Systems
Raj Shah - Koehler Instrument Company Inc.
Andrew Zheng - Koehler Instrument Company Inc.

With technological advancements, the demand for better lubrication is always increasing. Previous studies show that viscosity and vapor pressure play a major role in determining the usability of base oils. A combination of low vapor pressure and low viscosity is fundamental in creating new more efficient lubricating base oils. However, developing an oil that consists of these two properties is a challenge; as molecular weight decreases, vapor pressure increases and viscosity decreases which causes the oil to evaporate, leading to oil loss and environmental contamination. Polarity and isomerization are two oil properties that affect the oil evaporation and flow. These properties can be modified to adjust the flow activation entropy and intermolecular dispersion force to lower the viscosity while maintaining a low vapor pressure. This poster will compare results from various studies to explore the relationship between these properties for a series of hydrocarbon oils with a range of molecular weight and polarity as well as their isomers.

Abstract # 131 - Poster - 10/17/2018 - 1:00 PM - South Lobby

Orthogonal Selectivity for separation of light and heavy Petroleum Hydrocarbons by GCxGC

Ramkumar Dhandapani - Phenomenex

Complex sample mixtures including Petroleum hydrocarbons fractions requires detailed separation of individual class of organic compounds. A traditional GC approach will lead to multiple coelutions. In the present work, a GCxGC approach was considered to explore multi dimensional separation of complex light and heavier hydrocarbons. Due to high peak capacity in GCxGC, orthogonal selectivity of Zebron GC columns, complementary selectivity in 2 dimensions, a range of compounds including linear alkanes (n and iso-parafins),linear alkenes (olefins), cyclic alkanes, aromatics (one-ring teralin derivatives), Aromatics (one-ring, benzene derivatives), Aromatics (2-rings naphtalene derivatives), Aromatics (2-rings, dibenzene derivatives), Aromatic (3-rings), Aromatic (4-rings), Aromatic (5-rings)  were completely resolved. The column combination ZB-1HT and ZB-35 HT not only provided high temperature to elute all the fractions but also provided adequate selectivity to separate individual aliphatic and aromatics from each other.

Abstract # 132 - Poster - 10/17/2018 - 2:30 PM - South Lobby

Improved High Temperature Simulated Distillation (ASTM D6352 and D7169) Using Zebron™ ZB-1XT SimDist Metal GC Columns

Ramkumar Dhandapani - Phenomenex

An improved method for high temperature simulated distillation based upon ASTM D7169 is presented using the Zebron ZB-1XT SimDist column. This column utilizes a Glass Infusion™ Technology that results in more improved efficiency, resolution, and unmatched column-to-column reproducibility. This technology also allows simulated
distillation methods, such as ASTM D6352 and D7169, to be extended from C100 to C120 while still meeting all the system suitability requirements.Experiments show that the proven PDMS stability for boiling point based separation, high temperature resistance and faster equilibration not only provides good separation of hydrocarbon fractions but also provides reproducible results.

Abstract # 134 - Poster - 10/17/2018 - 11:30 AM - South Lobby

Cis- Trans FAME in Fuels by GC & GCxGC using ZB-FAME GC Column

Ramkumar Dhandapani - Phenomenex

Fatty Acid Methyl Esters (FAMEs) are a big threat in aviation fuels as well as in biofuels. Accurate quantitation and separation of cis trans, low and higher boiling FAMes is essential from quality control prespective as well as from a safety prespective. In the present work a ZB-FAME GC column is utilized to accurately characterize FAME in Fuels by GC MS. Traditional selectivity like a 100% Polyethyleneglycol phase may have few coelutions of FAME, while coupling ZB-Fame with Mass spec based detection priovides excellent separation of cis & trans FAME along with lower level detection. Traditional high cyano selectivity takes an hour to separate Cis/ trans FAMEs, while ZB-FAME can separate them within 11 min. This approach was also extended to 2D GC using ZB-Fame in the first dimension & a 5% phenyl selectivity in the second dimension to obtain orthogonal separation. Thus analysis of fuels by GC MS & GCxGC using  ZB-FAME  assures safety of aviation fuels.

Abstract # 140 - Poster - 10/17/2018 - 11:00 AM - South Lobby

Purity Measurement of Cyanogen Chloride using GC/MS and GC-ICP-MS

William Geiger - CONSCI, Ltd.

Cyanogen Chloride (aka CK) is compound that has been proposed for use in chemical warfare. It is a blood agent causing injury to the respiratory system and eyes. It is especially dangerous because it can penetrate many filters in gas masks. Because of this attribute, it is used as a test gas for evaluating gas mask filters. Government standards require 90% to 95% purity for test purposes. Conventional GC detectors are not capable of this quantitation accurately. Using GC/MS for identification and GC-ICP-MS for quantitation a comprehensive analysis can be accomplished.

Abstract # 153 - Poster - 10/17/2018 - 10:00 AM - South Lobby

Precision Comparison Between ASTM Sulfur Test Methods D7039, D2622, and D5453

Joseph Iaia - XOS
Leslie Johnson - XOS

Tighter regulations on sulfur concentrations have furthered the need for refineries to maximize the precision of their sulfur analysis methodology. Accurate measurements let refiners produce product closer to the specification maximums which saves money by reducing refining costs. With several methodology options for sulfur analysis available, refineries, terminals, and test inspection certification companies must take care to select a method that produces the least amount of variability. This paper reviews and discusses 3 years of ASTM PTP data for ULSD and RFG to compare test methods D7039, D2622, and D5453. The paper specifically takes a close look at the reproducibility results in the critical sulfur concentration range of 5 – 15ppm to determine which test methods offer users the least variability when running measurements according to the three ASTM methods of interest.

Abstract # 162 - Poster - 10/17/2018 - 10:00 AM - South Lobby

Diesel Fuels and Additives – Interference-free Determination of Total Sulfur with the Patented MPO Technology

Stefan Jezierski - Analytik Jena AG
Oliver Buettel - Analytik Jena AG

The determination of sulfur contents is an integral part of the process optimization and quality control in refineries, petro-chemistry and many other industry branches.
The most reliable and flexible method is the thermal decomposition with a subsequent UV fluorescence detection of the produced SO2 (EA). It is characterized by a superb detection sensitivity, long-term stability, and application flexibility. But there is one downside, the cross-sensitivity to NO. We describe a reliable technique for the interference-free sulfur determination. All measurements have been performed on compEAct SMPO elemental analyzer.

Abstract # 163 - Poster - 10/17/2018 - 10:30 AM - South Lobby

Analysis of Toxic Metals and TOC in Process and Waste Waters of the Petrochemical Industry

Bernd Bletzinger - Analytik Jena AG
Oliver Buettel - Analytik Jena

The petrochemical industry generates large volumes of waste water or effluents that must be treated before it can be reused or released into natural waterways. Toxic
heavy metals like Cadmium, Chromium, Lead and Mercury are typically monitored in process waters and effluents of petrochemical plants by Atomic Spectrometry range. Moreover, the total organic carbon (TOC) and the total bound nitrogen (TNb) content is routinely determined as these contaminants lead to eutrophication of surface water recourses, endangering aquatic life and ground water supplies.
For all these parameters the high concentrations of suspended solids (TDS) in waste waters can affect the direct analysis. Hence, the choice of the appropriate technique will depend on the digestion approach and sensitivity/throughput for TOC/TNb and AAS, ICP-OES and ICP-MS, respectively.

Abstract # 170 - Poster - 10/17/2018 - 10:00 AM - South Lobby

Total Sulfur and Nitrogen Analysis Using a Multi-Layer Combustion Tube

Anne Jurek - EST Analytical
Cory Black - EST Analytical

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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, 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 in light hydrocarbon samples using the NexiS combustion elemental analyzer complete with a new and novel multilayer combustion tube.

Abstract # 174 - Poster - 10/17/2018 - 10:30 AM - South Lobby

Detection of the Onset of Aggregation as a Function of pH of Iron Oxide Nanopowder by Dynamic Light Scattering

Lauren Szwast - Brookhaven Instruments Inc.

Given the great potential for applications using iron oxide, it is beneficial to understand the effect of chemical changes to the surface of the nanoparticle. The aim of this study was to determine if the onset of aggregation could be detected with a change in pH. The suspension was tested from a pH of 2 to 12 in 2 pH unit steps. The solution was analyzed using dynamic light scattering (DLS). The onset of aggregation was detected between pH 4 and 6. It was clear that as the pH value increased, the effective diameter increased and the stability decreased.

Abstract # 175 - Poster - 10/17/2018 - 11:00 AM - South Lobby

Micellar Water Characterization: A Laser Light Scattering Application

Dana Castro - Brookhaven Instruments

 When an aqueous solution has a certain amount of surfactant molecules, micelles are formed. The hydrophilic heads of the surfactant molecules orient themselves toward the water molecules while the hydrophobic tails orient towards each other, avoiding contact with water. These spherical aggregates are widely used in drug delivery, cosmetics, water treatment, detergents, and more. In order to determine if light scattering could be used to characterize commercial micellar waters, different brands were measured with laser light scattering. Size, charge, and rheological properties were all determined using a Brookhaven Instruments NanoBrook Omni. Results showed differences among brands and formulations.

Abstract # 196 - Poster - 10/17/2018 - 10:00 AM - South Lobby

OMNIS: Titration for Faster, Safer and Easier Analysis

Kerri-Ann Blake - Metrohm USA

Tight deadlines, high sample throughput, strict safety and quality standards – this is life in the analytical laboratory. This poster introduces the OMNIS titration platform that makes titration safer, faster and easier. We demonstrate the automation of four simultaneous analyses to increase sample throughput by 60% compared to existing methods. For safety, we describe a contact-free reagent exchange system that makes reagent exchange safer. Lastly, we show the safety and productivity benefits of this truly modular titration platform. Designed to grow with the needs of your laboratory, we present the OMNIS platform in expandable configurations that adjust to your laboratory demands.

Abstract # 197 - Poster - 10/17/2018 - 1:30 PM - South Lobby

Acid Number of Crude Oils and Petroleum Products by Catalytic Thermometric Titration using ASTM D8045

Kerri-Ann Blake - Metrohm USA
Lori Spafford - Metrohm USA

ASTM Standard D8045 describes the analysis of acidity in difficult crude oils and petroleum products using thermometric titration. This new technique overcomes solubility and precision challenges encountered with traditional potentiometric measurements. Thermometric titration is more precise, faster and reduces solvent requirements. Through eight years of development work in ASTM and thousands of sample measurements this new standard is shown to be rugged, robust and transportable across many labs and technicians. This poster provides a clear analysis of data acquired with this new method and details the benefits of thermometric titration for safer and more precise acidity analysis.

Abstract # 200 - Poster - 10/17/2018 - 10:00 AM - South Lobby

Determination of Total Fluorine, Chlorine, and Sulfur in Aromatic Hydrocarbons by Oxidative Pyrolytic Combustion Followed by Ion Chromatography (Combustion Ion Chromatography-CIC)

Carl Fisher - Thermo Fisher Scientific
Sachin Patil - Thermo Fisher Scientific
Jeff Rohrer - Thermo Fisher Scientific

The total fluorine, chlorine, and sulfur contained in aromatic hydrocarbon matrices can contribute to emissions that cause pollution, be harmful to many catalytic processes, and lead to corrosion. Ion chromatography (IC) is a sensitive and versatile method for the determination of halides and sulfate. Application of combustion IC (CIC), which combines oxidative pyrolysis with IC, has been demonstrated for many applications that determine the total amounts of these elements in samples. The work presented here describes determination of fluorine, chlorine, and sulfur in aromatic hydrocarbon samples based on ASTM method D7359-14a.

Abstract # 201 - Poster - 10/17/2018 - 10:30 AM - South Lobby

Fast Separation of Heat Stable Salts

Carl Fisher - Thermo Fisher Scientific
Manali Aggrawal - Thermo Fisher Scientific
Jeff Rohrer - Thermo Fisher Scientific

Hydrogen sulfide (H2S) and carbon dioxide (CO2) are often found in natural gas streams and are removed using amine-rich solutions before it can be transported/used. During this process, heat stable salts (HSS) can form as a result of an irreversible reaction of the amine with certain acidic components. Because HSS are corrosive, it is important that they be monitored. Here we present an Ion Chromatography (IC) method that uses a high-capacity, hydroxide-selective anion-exchange column with a fast gradient to analyze various refinery samples for the presence of common inorganic anions and heat stable amine salts.

Abstract # 206 - Poster - 10/17/2018 - 1:30 PM - South Lobby

Analysis of Oxygenates and Aromatics Using ASTM Method D4815 and D5580

David Scott - PerkinElmer
Lee Marotta - PerkinElmer
Leeman Bennington - PerkinElmer

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Gasoline samples are complex and a single column solution is not always readily available for the required analysis. As such solutions that have multiple columns, valves, backflushing and heartcutting ability have been developed to overcome these challenging separations. The resulting standardized methods can have a complex series of columns and valves that limit the flexibility of a gas chromatograph (GC) to analyze samples for other analytes. Removing and installing column sets is time consuming and causes instrument downtime with subsequent loss of productivity. Flexibility is a key attribute in the decision to purchase capital equipment for the increase in productivity and return on investment. The PerkinElmer Model ARNEL 4004 analyzer utilizes the same column set and valving for ASTM D4815 and ASTM D5580 enabling greater anaysis flexibility and subsequent return on investment.

Abstract # 208 - Poster - 10/17/2018 - 11:00 PM - South Lobby

Analysis of Total Petroleum Hydrocarbons (TPH) by GCxGC-FID

Matthew Edwards - SepSolve Analytical
Laura McGregor - SepSolve Analytical
Mark Lemons - Markes International
Aaron Parker - SepSolve Analytical

The determination of aliphatic/aromatic compounds when performing Total Petroleum Hydrocarbon (TPH) analysis is typically a lengthy process – with time-consuming sample fractionation and multiple analyses per sample.  

Here we show how the enhanced separation capacity of GCxGC-FID eliminates the need for offline sample fractionation.   

Furthermore, a dual-channel configuration can be used to double the sample throughput per instrument - increasing productivity, reducing bench space and lowering installation costs, all while meeting the criteria set out in standard methods (e.g. TPH Criteria Working Group and Massachusetts State).  

Abstract # 213 - Poster - 10/17/2018 - 2:30 PM - South Lobby

Analytical Sample Prep: The Forgotten Part of Method Development

Thomas Valorose - Pall Laboratory

High volume laboratories must keep instruments running while producing quality data. Using Pall Acrodisc syringe filters as part of the sample preparation process makes this possible by preventing column blockages without contributing extractable materials. Pall Acrodisc syringe filters increase HPLC column life 46 times and UHPLC columns over 111 times compared to unfiltered samples. Additionally, Pall Acrodisc syringe filters, with the four most common membrane chemistries, combine high particulate retention with minimal release of extractable materials. This makes them ideal for a variety of chromatography and sample preparation applications, including GC, ICP and specialized MS and ion chromatography techniques

Abstract # 222 - Poster - 10/17/2018 - 2:00 PM - South Lobby

Optimizing GCxGC Parameters for Petroleum Analysis using a Free Web-Based Tool

Christina Kelly - LECO Corporation
Joseph Binkley - LECO Corporation
Lorne Fell - LECO Corporation

Comprehensive two-dimensional gas chromatography (GCxGC) combined with time-of-flight mass spectrometry (TOFMS) is a well-established method for characterization of petroleum samples because of the ability to separate structural classes of hydrocarbons into distinct bands of analytes that can then be identified with library-matched mass spectra. However, transferring traditional one-dimensional gas chromatography methods to optimized two-dimensional methods can be daunting because of the sheer number of options available for setting up commercial GCxGC systems. Using a new online tool, SimplyGCxGC, the process of translating an existing analysis into an optimized GCxGC method is experimentally determined for a sample of diesel fuel.

Abstract # 227 - Poster - 10/17/2018 - 3:30 PM - South Lobby

Determination of Organochlorinated Components in Petrochemical Streams by XSD-GC (Halogen Specific Detector)

Leeman Bennington - PerkinElmer
Lee Marotta - PerkinElmer

The presence of organochlorinated components in petrochemical processes can form unwanted hydrochloric acid, ammonium chloride, and metallic chlorides resulting in corrosion, loss of catalyst efficiency, product impurities, and other process issues. Management of these components has grown in importance. Xylem’s XSD (halogen specific detector) is an exceptional tool to detect these bad actors. It uses no radioactive source, no organic solvents, and is simple to operate. This poster will demonstrate the use of the XSD and a PerkinElmer Clarus 680 GC for the analysis of organochlorinated components down to the sub-ppm range.

Abstract # 234 - Poster - 10/17/2018 - 2:00 PM - South Lobby

Identification of Oils by Synchronous Fluorescence Spectroscopy

Samantha Nania - PerkinElmer
Steve Upstone - PerkinElmer
Kathryn Lawson-Wood - PerkinElmer

Identifying and characterizing oil is vital for spill remediation. Crude oil and its distillates are fluorescent compounds and therefore can be analyzed using fluorescence spectroscopy. Specifically, a technique called synchronous fluorescence spectroscopy. This method utilizes both monochromators to simultaneously collect excitation and emission spectra at a constant difference to obtain a basic “fingerprint” for mixtures of fluorescent compounds such as these. 2D and 3D synchronous spectra (as constant wavelength synchronous luminescence) are used to show the fingerprint of three different samples, including aviation fuel, fuel oil, and Kuwaiti crude.

Abstract # 238 - Poster - 10/17/2018 - 10:30 AM - South Lobby

Determination of Organic Chlorides in Petroleum Products Using a Halogen Specific Detector (XSD)

Cynthia Elmore - OI Analytical

Recently there has been interest in the detection and removal of organic chloride species in petroleum products. Crude oil is distilled to form napthas and then this goes through catalytic reforming to produce reformates. Reformates are used for many products including gasoline blending stock and aromatic bulk chemicals so the process is crucial.1 During this process catalysts are conditioned with organic chlorides. If these are not removed they may form Hydrogen chloride and various organic chlorides which can cause operational problems such as corrosion and poisoning of downstream catalysts as well as product specification problems.2 Organic chlorides do not occur naturally in crude oils so when present they may be from contamination caused by equipment cleaning or used solvent disposal in dewaxing pipelines.3 Refineries see the need for a more comprehensive approach to the challenges that organic chlorides present in their processes.4 The ability to sample at various points in the process and speciate the organic chlorides is important to determine where the contamination is coming from and aids in evaluating processes and chloride removal. This poster will present a simple gas chromatographic method utilizing a halogen specific detector (XSD) to determine chlorinated organic compounds in various petroleum samples.

Abstract # 256 - Poster - 10/17/2018 - 10:00 AM - South Lobby

Applicability of micro packed columns (1/16“ x 1 mm id) packed with DiatoSorb solid support and configured for use in a dedicated capillary Agilent 6890 and 7890 GC.

Barry Burger - Restek Corp.

Columns and packings made with DiatoSorb solid support are superior in performance and reproducibility because Restek is the only global supplier that completely controls the physical and chemical properties of chromatographic-grade diatomaceous earth. This poster will demonstrate the performance, inertness, and speed of analysis obtained using Sulfinert-coated stainless steel micro packed columns (1/16 inch OD x 1 mm ID) compared to traditional packed columns (1/8 inch OD x 2 mm ID). The micro packed columns are easily installed and configured for on-column injection in a dedicated capillary Agilent 6890 or 7890 capillary GC as well as in a standard packed column GC.  

Abstract # 258 - Poster - 10/17/2018 - 2:00 PM - South Lobby

Solutions for analysis of FAME Biodiesel quality using gas chromatography

Katarina Oden - Restek
Barry Burger - Restek

Fatty Acids Methyl Ester (FAME) biodiesel is currently the most popular alternative fuel on the market. Biofuel burns cleaner and emits fewer greenhouse gases than traditional sources of energy. Therefore, it also makes for an environmentally friendlier option.  
FAME biodiesel is made from animal or vegetable fats with transesterification using acidic or basic catalyst and alcohol. All the steps of the reactions are strictly monitored and the final product is evaluated for reaction yields, residual starting materials, and byproducts. Presented will be solutions for determination of the final FAME content, residual alcohols, and glycerol/glycerides using gas chromatography.