2017 Posters

The following posters will be presented in the Exhibit Hall at the 2017 Gulf Coast Conference.

Abstract # 105 - Poster - 1/19/2018 - 9:30 AM - Exhibit Hall

Development of an NIR Analyzer for Measuring Multiple Fuel Properties of Commercial and Military Grade Jet Fuel in the Field

Dr. Raj Shah - Koehler Instrument Company
Cindy Galdamez - Koehler Instrument Company
Stuart Farquharson - Real Time Analyzers

When it comes to Aviation fuel of both commercial and military grade, quality and safety are of the utmost importance. A new technique has been developed for quick, in-field analysis of Jet Fuel properties that can be compared to the governing ASTM requirements. ASTM D1655 is the standard specification for aviation turbine fuels, the new portable near-infrared (NIR) analyzer that will be discussed in this poster can give results with comparable reproducibility to some of the key tests required by this standard. Before the development of this new technique, Raman spectroscopy was used to analyze several fuel properties, however these analyzers are very expensive and not feasible for commercial use. The new Portable Fuel Quality Analyzer uses optics, detectors, and a light source that are much more cost effective allowing there to be more fuel checks during the shipment process at fuel ports and depots. Through experimental research it was determined that an NIR analyzer that measures in the 1000 to 1600 nm spectral range with 5 nm resolution and a 1 cm path length would give results meeting ASTM repeatability and reproducibility for testing certain fuel properties. Through the use of multivariate statistics and a fuel sample data base the values given by the Portable NIR Analyzer were correlated to the ASTM proven values. Twenty-two correlation models for diesel, gasoline, and jet fuels were developed with the help of ASTM certified laboratories to compare repeatability and reproducibility values. The analyzer determined properties had reproducibility values that compared favorably to the ASTM values and the repeatability values of the analyzer properties often exceeded ASTM repeatability values. Therefore, for jet fuel in particular, the user can quickly and easily determine Density, API Gravity, Distillation Fractions, Flash Point, Viscosity (at -20°C), Freezing Point, Pour Point and Fuel System Icing Inhibitor values.

Abstract # 106 - Poster - 1/19/2018 - 9:50 AM - Exhibit Hall

Development of an ASTM Method to Reliably Predict Which Heavy Crudes or Petroleum Residua can be Mixed Without Causing Phase Separation

Dr. Raj Shah - Koehler Instrument Company
Cindy Galdamez - Koehler Instrument Company

The newly updated Automated Flocculation Titrimeter (AFT) automates the collection of Heithaus values and predicts flocculation for various crudes. It also allows users to easily and reliably predict which heavy oils and petroleum residua (including asphalts) can be mixed without causing phase separation. 

Typically, refiners all around the world have stopped processing crudes too soon because they couldn’t predict precisely when coking would occur. They’ve stopped well short of coke formation to avoid fouling in heavy oil processing equipment, tanks, and transfer lines but have reduced the distillate yield.  That is now history due to the development of the advanced AFT. This advanced laboratory tool is also capable of reverse titration and can be used for flocculation kinetic studies.

This expanded AFT methodology, now allows any refinery using this tool to recover additional distillate without fear of fouling. One can predict the refinery conditions for coking and stop processing before fouling occurs but not sooner than necessary by using the Coking Indexes pioneered by Western Research Institute. The AFT lets the user quickly and easily collect the data needed for analysis.

The theory behind this innovative technique is discussed in this poster as well. Petroleum residua consists of ordered structures of associated polar asphaltene complexes that are dispersed in a lower polarity solvent phase by intermediate polarity material commonly referred to as resins. When the residuum is heated to temperatures above 340 degrees Celsius, this suspended structure is systematically and irreversibly destroyed during pyrolysis. A common problem in the refining industry is to ascertain how close a pyrolysis system is to forming coke on the coke induction period timeline. A certain amount of pyrolysis typically occurs and can be tolerated in a distillation unit, since there is an induction period prior to the appearance of coke.

The automated flocculation titrimeter has been developed to perform ASTM D6703, the official test method for automated Heithaus titrimetry. This helps to measure the state of the dispersed particle system and calculates predictive parameters for heavy oils.

The advanced AFT can now be used to provide valuable information about the internal stability of a heavy oil, the proximity of a pyrolyzed oil to coke formation, and to design blending protocols for oils mixtures related to prevent asphaltene precipitation, as well as study flocculation kinetics. It is an extremely versatile tool for the petroleum industry in both upstream and downstream operations.

Abstract # 109 - Poster - 1/19/2018 - 1:00 PM - Exhibit Hall

Development of an Energy Dispersive X-ray (EDXRF) Technology and Experimental Technique to Measure Low PPM of Sulfur and Chlorine to Comply with Tier 3 Gasoline Standards

Dr. Raj Shah - Koehler Instrument Company
Vincent Colantuoni - Koehler Instrument Company
Eric Cervino - Koehler Instrument Company

Starting 2017- barring any last minute revisions- the Environmental Protection Agency (EPA) will be administering new Tier 3 Gasoline Standards. In the latest, compelling attempt to reduce air pollution, the new standards will affect high sulfur content in gasoline to promote cleaner emissions from passenger vehicles and trucks. To comply with the new requirements set in place, fuel composition must now be limited to a maximum of 10 ppm sulfur content.  

ASTM D7220 “Standard Test Method for Sulfur in Automotive, Heating, and Jet Fuels by Monochromatic Energy Dispersive X-ray Fluorescence Spectrometry” can be used to verify various fuels’ compatibility with the newly implemented EPA standards. Types of fuels covered under ASTM D7220 include oxygen-enriched gasoline (RFG), diesel, diesel/biodiesel blends (volume ≤ 20% biodiesel), kerosene, jet fuel, jet fuel/biodiesel blends (volume ≤ 5% biodiesel) and No. 2 home heating oil. This poster will focus mainly on experiments conducted with gasoline, however. The test method’s assignment is based off evidence proving that current EDXRF (Energy-Dispersive X-ray Fluorescence) Technology using matrix-matched empirical calibrations can be used for the EPA performance-based testing.

Koehler’s EDXRF apparatus adheres to the ASTM D7220 model and has been manifested to ensure a refiner meets with the newly enforced Tier 3 Gasoline Standards and the associated robust regulations. After numerous rounds of laboratory testing, the ASTM D7220 test method has a proven record of accurately measuring the presence of sulfur in various fuel samples. This powerful analytical tool utilizes polarized X-ray technology to accurately determine the sulfur content of the sample in question. When the beam passes through the sample, it reveals the sulfur content after comparing it to a sulfur-free background spectrum. By using the Koehler EDXRF instrument, refiners can be confident in their continued compliance with the EPA by providing the agency with accurate, reportable data. Preliminary data along with results and discussion will be included in our findings.

Abstract # 110 - Poster - 1/19/2018 - 11:10 AM - Exhibit Hall

Construction and Evolvement of a State of the Art Laboratory Technique for Corrosion Measurement: Comparative Study of a Variety of Samples Using NACE/ASTM D665 in Relation to a New Benchtop Accelerated Corrosion Test Method

Dr. Raj Shah - Koehler Instrument Company
Imran Husseni - HollyFrontier Refining
Vincent Colantuoni - Koehler Instrument Company
Eric Cervino - Koehler Instrument Company

The muddled composition of some petroleum products contain elements that cause corrosion on interior surfaces, leading to the degeneration of pipelines and formation of detrimental deposits inside engines. The method used for analyzing the corrosive properties of gasoline and distillate fuels in preparation for transport through a pipeline was originally developed by the National Association of Corrosion Engineers. The NACE TM0172 test method requires four hours to produce results and demands a 300mL sample of the product in question. While this test method's success has served the industry well for many years, key stakeholders began expressing a profound interest for an improvement exhibiting a faster turnaround and smaller sample size requirement to promote better repeatability and reliability. Working closely with key refineries around the country and executing numerous extensive laboratory trial and error experiments has all lead to a faster, easier, and more reliable test method. The new ASTM test method, ASTM D7548 for Determination of Accelerated Iron Corrosion in Petroleum Products is the evolution in state of the art laboratory corrosion measurement procedures. Its revolutionary characteristics touches upon some engineering concerns expressed by industry leaders regarding the accelerated corrosion test methods of the past. The new method only requires a 50mL sample and less than a fourth of time to complete testing in comparison to the NACE TM0172 and ASTM D665 accelerated corrosion test methods. This less demanding laboratory setup will save the industry significant time when testing to determine the corrosive qualities of various petroleum products. When applied to pipeline transfer station operations- where a quick QC turnaround time is absolutely critical- the ASTM D7548 test method becomes an adequate substitute for assurance. This poster will discuss the comparative data originating from preliminary instrument testing.

Abstract # 116 - Poster - 1/19/2018 - 9:30 AM - Exhibit Hall

Lubricating Oils Analysis Using Thermal Desorption and Pyrolysis / Direct Analysis in Real Time-Mass Spectrometry (TDP/DART-MS)

Chikako Takei - BioChromato, Inc.
Kenichi Yoshizawa - BioChromato, Inc.

Lubricating oils are composed of base oil and additives. To satisfy the high specific demands accompanying the development of machinery and automobiles, synthetic base oils and various additives are used. Generally, since complicated pre-treatment is necessary for analysis, extending the time and increasing the effort required to obtain results. If analysis without pre-treatment is possible, it will be useful for research and development. We conducted this study using TDP/DART-MS without any pre-treatment. Additives and base oil in the lubricating oils were analyzed respectively. Moreover, this analysis method could be applied to evaluate the degradation degree. 

Abstract # 129 - Poster - 1/19/2018 - 1:20 PM - Exhibit Hall

A Detailed Study and Comparison of a Variety of Bench Scale ASTM Oxidation Tests for Lubricating Oils

Nicole Passariello - Koehler Instrument Company, Inc.
Dr. Raj Shah - Koehler Instrument Company, Inc.
Vincent Colantuoni - Koehler Instrument Company, Inc.

Various ASTM test methods are currently used to test the oxidation properties of lubricating oils. They vary based on the type of lube oil they are attempting to test and the aim is usually to emulate under laboratory conditions, the real world conditions that the oils are subjected to. The primary factors that are usually available in the lab to simulate such a real life condition are the duration of the test, the temperature the sample is subjected to, catalyst that can be used to speed up the oxidation process, the atmosphere and condition under which the sample is tested etc. By changing these conditions for different kinds of oils, various ASTM oxidation tests have been created to study the oxidation and thermal performance of lubricants in the laboratory. Some of the lubricating oils that ASTM accounts for in their oxidation testing include hydraulic, R&O, turbine fuel oils, gear oils, greases, engine oils etc..  The test methods include ASTM D 942 - Oxidation Characteristics of Inhibited Mineral Oils, ASTM D 2893 - Oxidation Characteristics of Extreme Pressure Lubricating Oils, and ASTM D 5763 - Oxidation and Thermal Stability Characteristics of Gear Oils Using Universal Glassware just to name a few. The goal of this study is to look at these various test procedures already developed, and to attempt to create a more universal procedure / apparatus that can be modified by the user in their laboratory to run their own research protocols, while developing newer and longer lasting lube oils.

Abstract # 138 - Poster - 1/19/2018 - 10:00 AM - Exhibit Hall

Fast Simulated Distillation Analysis by Modified ASTM® D2887, D7169, D6352, and D7500

Tracy Dini - Perkin Elmer Inc.
Mamdouh Farag - Perkin Elmer Inc.

Simulated Distillation (SimDis) is a GC technique used to simulate the results of a distillation tower, separating crudes into component fractions by boiling points. The PKI Dragon software takes the chromatogram of the crude oil sample and correlates it with a calibration performed on known parrafins comparing RT to BP and calculating the SimDis result. To obtain this result in a short time the GC is pushed to its maximum operating temperature. The Perkin Elmer Clarus 690GC equipped with a POC Injector and Wide Range FID is built to withstand this high performance level while providing optimal sensitivity. Knowing the product fractions of crude oil ahead of time allows adjustments to be made to the refining process, resulting in higher efficiency rates of distillation for the crude oil. 

Abstract # 142 - Poster - 1/19/2018 - 11:00 AM - Exhibit Hall

Development of Ion Chromatography and Mass Spectrometry Technique for Squeeze Management

Lei Cheng - Ecolab
Christopher Durnell - Ecolab
Emerils Casado-Rivera - Ecolab

Aminophosphonates are effective scale inhibitors used to prevent and control scale problems in oilfields. It is significant to measure the accurate and precise scale inhibitor residuals to manage the squeeze treatment. The prevalent analytical technique inductively coupled plasma Optical Emission Spectroscopy (ICP-EOS) is simple and used to quantify aminophosphonate by measuring the phosphorus content in the sample. However, it is not able to differentiate phosphonate mixtures in the commingled sample. In this work, we developed ion chromatography and triple quadrupole mass spectrometry (e.g. IC-MS and IC-MS/MS), which have high sensitivity and specificity to quantify several phosphonates in the system. Ion chromatography efficiently separates phosphonate ions from other salt ions, because phosphonates are multivalent anions which have the stronger interaction with the column than the monovalent chloride anions or other anions. At an early stage, the IC-MS method has been developed to differentiate two phosphonates in the squeeze treatment. As the increase of the complexity of the squeeze treatment, more advanced technique, IC-MS/MS has been developed to differentiate four phosphonates in the commingled sample. The innovative technique can detect the low level of phosphonate in the mixture at 1 ppm. The technique has been validated using synthetic brine and field brine. The IC-MS/MS method is a powerful technique in squeeze scale management. In future, further analysis of real field samples of the squeeze treatments of multiple wells will be performed.  

Abstract # 143 - Poster - 1/19/2018 - 10:20 AM - Exhibit Hall

GC-ICP-MS Analysis of Nickel and Iron Carbonyl in Carbon Monoxide and Syngas

William M. Geiger - CONSCI, Ltd.
Jesus Anguiano - CONSCI, Ltd.
Blake McElmurry - CONSCI, Ltd.

GC-ICP-MS Analysis of Nickel and Iron Carbonyl in Carbon Monoxide and Syngas Carbon monoxide is an important industrial gas with a wide variety of uses. It is present in many gas mixtures such as Syngas and even mixed with natural gas.  Presence of metal carbonyls, particularly nickel and iron can be problematic when gas is used as fuel, semi-conductor modifier, or as a therapeutic medical gas.  Heretofore analytical methods have been suspect due the difficulty in calibration and the labile/reactive nature of the analytes.  A novel approach has been developed for accurate analysis using GC-ICP-MS.

Abstract # 153 - Poster - 1/19/2018 - 10:40 AM - Exhibit Hall

Dual-Channel GC×GC-FID for Routine TPH Analyses

Chris Hall - SepSolve Analytical
Matthew Edwards - SepSolve Analytical
Laura McGregor - SepSolve Analytical
Aaron Parker - SepSolve Analytical
Nick Bukowski - 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 # 155 - Poster - 1/19/2018 - 11:00 AM - Exhibit Hall

Unlocking the Power of GCxGC: Advances in Data Processing Workflows

Matthew Edwards - SepSolve Analytical
Laura McGregor - SepSolve Analytical
Chris Hall - SepSolve Analytical
Nick Bukowski - SepSolve Analytical

GCxGC forms the ideal platform for analysis of complex mixtures, but there is often the preconception that it involves time-consuming data processing.

ChromSpace software provides fast and efficient data processing by enabling sophisticated peak merging, simple group-type analysis and efficient scripting for target species

Here we will demonstrate simple yet effective GC×GC data processing for a range of file types, proving that this technique can be a productive contributor of any high-throughput laboratory.

Abstract # 157 - Poster - 1/19/2018 - 10:00 AM - Exhibit Hall

Determination of Chlorinated Compounds in Hydrocarbon Streams Using a Halogen Specific Detector(XSD)

Cynthia Elmore - OI Analytical

There has been an increase in concern for the detection and removal of organic chloride species from crude aromatic streams, naptha streams, and other hydrocarbon streams. One process called catalytic reforming uses organic chloride to condition the catalyst which results in low level chloride contamination downstream. This can take the form of hydrogen chloride (HCl) and organic chlorides. The chloride species can cause a number of problems in the various refining processes including formation and deposition of ammonium chloride, corrosion, poisoning of catalysts, and fouling of product. Since reformates and other aromatic and naptha streams are used to make gasoline blending stock, aromatic bulk chemicals, and raw materials for plastics, determining and removing contaminants is essential. Analysis by the halogen specific detector (XSD) can be useful in the detection of organic chlorides. This detector offers advantages over other halogen selective detectors such as, it contains no radioactive source, doesn’t use organic solvents, and is simple to operate. This poster will show a method for organic chloride analysis with a representative compound list and a calibration range of 0.1 to 50ppm.

Abstract # 161 - Poster - 1/19/2018 - 11:20 AM - Exhibit Hall

FAMEs Analysis In Less Than 12 Minutes! Reducing Analysis Time Using The Magic Of GC Column Parameters

Ramkumar Dhandapani - Phenomenex
Timothy Anderson - Phenomenex
Marc Gregerson - Phenomenex

 Increased resolution and efficiency are every analytical chemist’s desire. Though a 60 minute analytical run has traditionally been common for analysis of fatty acid methyl esters (FAMEs) due to their unique structures, analysts in production environments often mention the need for faster run times to improve productivity. Using several key GC column parameters including selectivity and dimensions, run time for a typical 37 component FAMEs sample can be reduced to as short as 12 minutes. Using a high-cyano Zebron™ ZB-FAME GC column, demonstrated a successful tactics for achieving short run time, successful FAMEs testing methods for real samples.

Abstract # 164 - Poster - 1/19/2018 - 1:20 PM - Exhibit Hall

Accurate Analysis of Low-Level Sulfur Compounds Using Gas Chromatography Coupled with a Sulfur Chemiluminescence Detector

Jim McCurry - Agilent Technologies
Jason Ashe - Agilent Technologies
Paul Barboni - Agilent Technologies

Being able to measure sulfur compounds reliably and routinely is of utmost importance to the petrochemical industry.  For liquid petroleum analysis, sulfur-containing compounds are present in petroleum feed stocks and are monitored during the refinement process to effectively maintain downstream processing.  In natural and petroleum gases, sulfur may be naturally occurring or added for safety purposes. 

A gas chromatograph equipped with a sulfur chemiluminescence detector (SCD) provides rapid and efficient means for quantifying sulfur compounds from various processes. SCDs provides linear responses to sulfur-containing compounds with improved detector stability and minimal hydrocarbon interference. 

For this experiment the detector was combined with an Agilent 9000 Intuvo gas chromatograph (GC) which provides a smaller footprint, inert flow path, direct heating technology, and click-and-run connections.  The inert flow path allowed for repeatable and quantitative transfer for 22 sulfur containing compounds from ranging from 100ppm to 0.1ppm.  For light petroleum liquids, the average area repeatability was found to be 4.1% for the 0.1ppm standard (0.01 ppm on-column due to a 10:1 split) and improved to 3.2% or better for the higher concentrations.  The coefficient of determination was found to be 0.999 for >80% of the analytes evaluated. 

The practical limit of detection for this application was determined by injecting a 20ppb standard split 10:1. Most the 22 analytes were differentiated from baseline noise at this level indicating a practical limit of detection of 2ppb. Analysis of natural gas samples on an Intuvo GC equipped with a gas sampling valve will also be presented. The click-and-run connections on the GC improves the user experience and simplifies method development by enabling quick column changes. This highly stable system with an innovative inert flow path that greatly simplifies and improves the analysis of sulfur-containing compounds.  

Abstract # 170 - Poster - 1/19/2018 - 11:00 AM - Exhibit Hall

New High Temperature PEG GC Column with Increased Temperature Limit and Ultra-Low Bleed Level

Vanessa Abercrombie - Agilent Technologies
Ngoc-A Dang - Agilent Technologies
John Oostdijk - Agilent Technologies
Frans Biermans - Agilent Technologies
Laura Provoost - Agilent Technologies
Daron Decker - Agilent Technologies
Phil Stremple - Agilent Technologies

WAX columns based on 100% Polyethylene Glycol stationary phase are used for the analysis of a variety of compounds, such as industrial chemicals, but often suffer from a limitation of upper temperature limit, mainly up to 250°C/260°C and high bleed level resulting in low sensitivity, low reproducibility, poor column lifetime and increased analysis time. The new High-Temperature WAX (DB-Heavy Wax) GC column, has an extended upper temperature limit, up to 280°C/290°C and decreased bleed. In comparison to other Wax columns the DB-Heavy Wax shows superior performance for thermal stability at extended upper temperature limit, increased reproducibility, and improved column lifetime.

Abstract # 174 - Poster - 1/19/2018 - 11:00 AM - Exhibit Hall

Determination of Absorbable Organic Halogen in Wastewater

Carl Fisher - Thermo Fisher Scientific
Jingli Hu - Thermo Fisher Scientific
Jeffrey Rohrer - Thermo Fisher Scientific

Absorbable organic halogens (AOX) are an indicator of industrial water pollution. The AOX are defined as the fluorine, chlorine, and bromine compounds absorbed from water by activated carbon. To measure the AOX we applied combustion ion chromatography. The activated carbon containing the AOX was combusted in an oxygen atmosphere by an automated combustion instrument. The resulting gas was trapped in an absorbing solution, where fluoride, chloride, and bromide represent the water’s organic halogens. A portion of the absorbing solution was automatically transferred to an ion chromatography system to measure the halogen anions. This method accurately measured AOX in wastewater.

Abstract # 181 - Poster - 1/19/2018 - 1:40 PM - Exhibit Hall

Enhanced Quantitation and Reporting Features for ASTM D5769 Using ChromaTOF-BT

Christina Kelly - LECO Corporation

Creating fully customizable reports that meet the variety of needs outlined in the ASTM D5769 Standard Test Method for Determination of Benzene, Toluene, and Total Aromatics in Finished Gasolines by Gas Chromatography/Mass Spectrometry can be a challenge. With ChromaTOF-BT, fully integrated hardware control, data processing, and reporting features are combined with new quantitation types to allow a seamless experience that exceeds method criteria. From collecting wide linear dynamic range, full-mass-range time-of-flight mass spectral data to reporting deconvoluted peaks, ion ratio results, and using multiple internal standards, the LECO Pegasus BT system operating on ChromaTOF-BT provides an excellent solution for a variety of established methods, including ASTM D5769.

Abstract # 184 - Poster - 1/19/2018 - 9:50 AM - Exhibit Hall

Analysis of Light Hydrocarbons Using a Single-Plate Reverse Fill/Flush GC x GC Differential Flow Modulator

James D. McCurry - Agilent Technologies, Inc.
Jason Ashe - Agilent Technologies, Inc
Jim Luong - Dow Chemical Canada
Shi-Fen Xu - Agilent Technologies, Inc
Taylor Hayward - Dow Chemical Canada
Juan Aybar - Agilent Technologies, Inc
Roger Firor - Agilent Technologies, Inc
Matthew Giardina - Agilent Technologies, Inc

Flow modulated comprehensive two-dimensional gas chromatography is a rugged and low cost alternative to cryogen-based thermal modulators.  Construction of a diffusion bonded single-plate device can further enhance simplicity and robustness by incorporating an internal collection channel, projection welded gas connections, and leak-free metal ferrule column connections.  The device is well suited for the analysis of permanent gases and light hydrocarbons which are too volatile to be trapped efficiently using thermal modulation.  In this paper, the separation of light hydrocarbons is demonstrated using a single-plate reverse fill/flush differential flow modulator with PLOT columns.

Abstract # 192 - Poster - 1/19/2018 - 10:00 AM - Exhibit Hall

Advantages of Temperature Controlled Sample Introduction for High Volatile and Viscous Organic Samples with ICP-OES

Nora Bartsch - Thermo Fisher Scientific (Bremen) GmbH
Dr. Elena Chernetsova - Thermo Fisher Scientific (Bremen)
Paul Voelker - Thermo Fisher Scientific

Temperature stability of the sample introduction can be a major concern when it comes to reproducibility of analysis results. In addition, the temperature of the introduced sample also plays a role in the sensitivity of the instrument. The ability to control the temperature of the introduced sample leads to more control of the changes of the sample properties, to be able to introduce high volatile and viscous samples and low volumes.

Abstract # 195 - Poster - 1/19/2018 - 11:00 AM - Exhibit Hall

Chloride Monitoring in Feedstocks and Process Streams Using MWDXRF

Kyle Kuwitzky - XOS

The presence of chlorides in crude feedstocks and process streams can cause billions of dollars in lost profits due to corrosion at petroleum refineries. Chlorides are not naturally occurring in crude and are introduced by contamination during transportation or brine from a well. Refineries are implementing MWDXRF to allow for monitoring of sub-ppm chlorine content in the feedstocks and process streams. This enables the refineries to implement strategies that greatly reduce the costs of corrosion.

Abstract # 200 - Poster - 1/19/2018 - 10:30 AM - Exhibit Hall

Process Raman Spectroscopy in Polymer Manufacturing

Patrick Wiegand - Kaiser Optical Systems Inc.
Jeremy Linoski - Kaiser Optical Systems Inc.
Tim Felder - Felder Analytical
David Strachan - Kaiser Optical Systems Inc.

Raman spectroscopy is a versatile technique in measuring and controlling polymer processes. In a process environment, an on-stream Raman analyzer can improve process knowledge and enable in-process corrections. We present Raman applications in polymers which include polymerization blending, extrusion monitoring, crystallinity, and copolymers. Raman spectroscopy can be coupled to rheometry, enabling simultaneous collection of chemical and rheological properties. Biological polymers and plant-based polymers are emerging applications within the polymer industry. We show examples where the use of Raman spectroscopy has been shown to improve understanding of polymer chain entanglement, polyethylene density, polymer blend composition, or monomer concentration during production.

Abstract # 202 - Poster - 1/19/2018 - 10:00 AM - Exhibit Hall

Real Time Process Optimization to Meet Sulfur and Nitrogen Regulatory Challenges

Lisa Houston - PAC

In the US and around the world, refiners must be able to measure the precise amount of sulfur and/or nitrogen in their intermediates and products in real time, so they know what needs to be done to optimize the product so that it is as close to the specification as possible saving money and extending the life of the catalyst(s). Refiners can also use these measurements to optimize the process to create the most cost-effective blend that meets the final sulfur requirements of the product.  Meeting these requirements is costly for many reasons. Crude oil is becoming more sour, so the amount of sulfur in the crude is increasing, requiring more processing. In addition, regulations that apply to the end products are also increasingly challenging.  This paper will discuss applications of an improved process elemental analyzer designed to meet the challenge of measuring sulfur and/or nitrogen in a wide range of materials including sulfur in gasoline to meet the EPA Tier 3 gasoline and Ultra Low Sulfur Diesel (ULSD) regulations, sulfur content in marine fuel to meet International Marine Operations (IMO) SECA regulations and nitrogen and sulfur in heavy diesel for low and medium speed diesel engine applications involving primarily constant speed and load.

Abstract # 203 - Poster - 1/19/2018 - 10:00 AM - Exhibit Hall

Overcoming Challenges in Heavy Oil Viscosity Management

Dan Airey - PAC
Jonathan Cole - PAC

There are more than 700 refineries worldwide with a capacity for 82 million barrels of oil per day. A barrel of crude yields gasoline, fuel oil, jet fuel, diesel, asphalt, lubrication oil and other refined products, but actual output varies dramatically by refinery. Viscosity is one on the most critical measures of product quality, for all product types. Heavy oils are traditionally the most difficult to work with and manage. This presentation will discuss how heavy oil producers are turning to the latest developments in viscosity management to improve quality, cost, and output while minimizing equipment downtime and maintenance.

Abstract # 206 - Poster - 1/19/2018 - 10:20 AM - Exhibit Hall

Improved Process Blending Through Micro Distillation

Henry Montoya - PAC

The U.S. Environmental Protection Agency (EPA) has approved the use of E10 (90% gasoline/10% ethanol) fuels in light duty vehicles.  Fuel grade ethanol is blended in nearly all of the nation’s conventional E10 and reformulated gasoline as well as other blends such as E85 (85% gasoline/15% ethanol).     Fuel quality regulations and specifications vary by state. Some may adopt all or a portion of ASTM D4814 Standard Specification for Automotive Spark-Ignition Engine Fuel and require any ethanol blended into gasoline meet ASTM D4806 Standard Specification for Denatured Fuel Ethanol for Blending with Gasolines for Use as Automotive Spark-Ignition Engine Fuel. With constant changes in quality and the composition of the fuels available, hitting the ultimate blend target is a significant challenge.  A primary physical property parameter for gasoline is distillation, according to ASTM D86 Standard Test Method for Distillation of Petroleum Products and Liquid Fuels at Atmospheric Pressure or the equivalent ASTM D7345 Standard Test Method for Distillation of Petroleum Products and Liquid Fuels at Atmospheric Pressure (Micro Distillation Method). Continuous process data has proven to help blenders optimize the blend variables to hit the fuels target and still be in compliance with environmental authorities.    This poster discusses the use of Micro Distillation in a process, for improving ethanol blending in gasoline by providing a full distillation curve, every 10-12 minutes, while correlating to the traditional D86 results.

Abstract # 217 - Poster - 1/19/2018 - 9:50 AM - Exhibit Hall

What’s New at ASTM? Moving Method D3606 from Packed to Capillary Technology

Leeman Bennington - PerkinElmer
Lee Marotta - PerkinElmer

The EPA regulates the amount of benzene in gasoline specifying ASTM method D3606-10. The resolution of benzene from ethanol using this packed column method is a challenge. The ubiquitous use of ethanol as a blend component of gasoline makes it necessary to improve the method. In addition, butanol has been approved for use in gasoline which the scope of D3606-10 does not cover.

PerkinElmer has revised D3606 to capillary technology enhancing the resolution and accuracy of benzene for oxygenated blends.

This presentation provides updates from the ASTM ILS steering committee leader including method parameters, validation studies and future status of the improved method.

Abstract # 225 - Poster - 1/19/2018 - 11:00 AM - Exhibit Hall

Meeting TIER III Performance Based Measurement System Criteria for Measuring Low Level Sulfur by ASTM D5453 in Automotive Fuels

Robbert Van Wessel - PAC lp

The United States environmental protection agency (EPA) has introduced a new program to control the air pollution from motor vehicles. This program is called the TIER III and is further limiting the emission of sulfur content in automotive fuels to a maximum of 10 ppm(w) total sulfur content. With the previous TIER 2 program the Performance-Based Measurement System (PBMS) approach was introduced and this will now become mandatory. To comply with the PMBS regulation site precision and accuracy of the analyses technique needs to be monitored and evaluated constantly on site.   Typical data will be presented for measuring low level sulfur concentrations in gasoline samples per ASTM D5453 with complying to the new TIER III criteria.

Abstract # 235 - Poster - 1/19/2018 - 9:50 AM - Exhibit Hall

The Analysis of Distillate Products per ASTM D8110-17 Using the Agilent 7800 and Teledyne-Cetac MVX-7100 µL Autosampler

Lindsey Whitecotton - Agilent Technologies
Jenny Nelson - Agilent Technologies

Stringent specifications in the petroleum industry requiring more sensitive measurements led to the new standard test method, ASTM D8110-17, utilizing ICP-MS. Multiple distillate products were analyzed per ASTM D8110-17 on an Agilent 7800 ICP-MS, using the syringe driven, septum piercing MVX-7100 µL autosampler.

Abstract # 236 - Poster - 1/19/2018 - 11:40 AM - Exhibit Hall

Selective Analysis of Trace Level Carbonyl Sulfide in Propylene by Gas Chromatography and Chemiluminescence as Alternative Detection for ASTM D5303

Marijn Van Harmelen - PACLP
Rob De Jong - PAC

In processes producing propylene, trace level carbonyl sulfide (COS) acts as a poison to commercial polymerization catalysts, resulting in deactivation and costly process downtime. The PAC SeNse Chemiluminescence Detector is the most advanced GC Detector available for the selective determination of sulfur containing compounds in hydrocarbon matrices. Typical data will be presented for the analysis of carbonyl sulfide in propylene by Gas Chromatography and chemiluminescence detection.

Abstract # 262 - Poster - 1/19/2018 - 10:30 AM - Exhibit Hall

A New Approach for Analyzing Water in Petroleum Products

Mark Janeczko - Shimadzu Scientific Instruments, Inc.

Water in petrochemical feedstocks can cause problems for processors. Freezing of pipe lines and valves and poisoning of expensive catalysts are just a few examples. Monitoring water in petroleum from an upstream source to the downstream processing plant is critical to insure uninterrupted operation. Unlike the commonly used Karl Fischer Titration analysis technique, the Shimadzu water analysis method uses the unique GC/BID and Merck’s WaterColTM eliminating the adverse effects of the petroleum matrix which can skew the Karl Fisher results. This method provides sensitive and accurate results in concentrations from low ppm to 100%.

Abstract # 263 - Poster - 1/19/2018 - 10:20 AM - Exhibit Hall

Shimadzu simulated distillation system, Nexis GC-2030 and LabSolutions SIMDIS

Satoshi Yano - Shimadzu Corp.

Simulated distillation analysis utilizes a gas chromatograph equipped with a nonpolar column for the boiling-point distribution analysis of petroleum fractions, such as kerosene, diesel oil, and heavy oil.

Shimadzu's new high-end gas chromatograph, Nexis GC-2030, offers a modern approach to a classic chromatographic technique.
Shimadzu's simulated distillation system, Nexis GC-2030 and LabSolutions SIMDIS, meets all applicable ASTM, ISO, EN, and JIS standards and enables the accurate and highly reproducible analysis of high-boiling components in crude oil samples.
It is the optimal system for product quality control and process management in oil refinery plants.
LabSolutions SIMDIS is an optional add-on for LabSolutions. It includes several functions commonly used for the calculation of distillation characteristics of various petroleum distillates.
Here we introduce the SIMDIS software and some results.

Abstract # 271 - Poster - 1/19/2018 - 1:40 PM - Exhibit Hall

Versatile sampling approaches compatible with Thermal desorption pre-concentration for analysis of VOCs & SVOCs in environmental samples

Lara Kelly - Markes International Ltd
Massimo Santoro - Markes International Ltd
Wade Bontempo - Markes international ltd
Ben Landas - Markes international ltd
Nicola Watson - Markes International ltd

Analysis of volatile/semi-volatile organics in environmental samples often requires extensive sample preparation for extraction/concentration of target analytes.  Thermal desorption has commonly been employed as a ‘solvent-free’ approach for environmental air-monitoring, but has historically been limited in its ability to deal with matrices such as liquids and solids.

In this poster, we describe High-capacity sorptive extraction and compare it with other sampling approaches compatible with TD–GC–MS.  These are applicable to a number of environmental samples including PAHs and fuel contaminated soil samples.

These studies use a new generation of thermal desorbers with outstanding capabilities for these challenging analytes.

Abstract # 272 - Poster - 1/19/2018 - 1:40 PM - Exhibit Hall

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

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 # 273 - Poster - 1/19/2018 - 2:00 PM - Exhibit Hall

OMNIS: Titration for Faster, Safer and Easier Analysis

Lori Spafford - 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 analysis 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 # 288 - Poster - 1/19/2018 - 10:30 AM - Exhibit Hall

Passive Monitoring – A Guide to Sorbent Tube Sampling for EPA Method 325

Nicola Watson - Markes International
Wade Bontempo - Markes International
Matt Edwards - Markes International

US EPA Method 325 has been developed to enable refineries to comply with the updated US federal regulation CFR 40, and requires monitoring of VOCs around the boundary of refineries. This involves two-week passive (diffusive) sampling onto sorbent tubes, followed by analysis by thermal desorption (TD) in conjunction with gas chromatography (GC), with analysis by mass spectrometry (MS) or other detection technique.

While benzene is the primary target compound, the sampling and analysis methodology can also be used to determine other VOCs, including butadiene, toluene, ethylbenzene, xylenes and other hazardous air pollutants (HAPs). This paper will explain the stepwise process of the method and discuss how innovative sampling and analytical instrumentation is used to fully comply with Method 325.

Abstract # 290 - Poster - 1/19/2018 - 9:30 AM - Exhibit Hall

Improving the Analytical Sensitivity and Overcoming Chromatographic Coelution in the TO-15 GC-MS Method for Measuring Air Toxics

Ngee Sing Chong - Middle Tennesse State University
Kiin Keith - Middle Tennessee State University
Archana Tirumala - Middle Tennessee State University
Xintian Yu - Middle Tennessee State University

Development of a highly sensitive analytical method for the analysis of gaseous volatile organic compounds (VOCs) is critical to the air quality monitoring program of regulatory agencies, environmental testing laboratories, and atmospheric chemistry research. A gas chromatography-mass spectrometry (GC-MS) based on cryogenic preconcentration of analytes and the use of simultaneous scan and selected ion monitoring (SIM) modes was used to characterize the distribution and concentrations of ambient air toxics in Memphis. Both the Automatic Mass Spectral Deconvolution and Identification System (AMDIS) and TargetView programs were compared for their ability to correctly identify co-eluted compounds.

Abstract # 300 - Poster - 1/19/2018 - 10:00 AM - Exhibit Hall

Overcoming Challenging SM 5310B TOC Determinations of Municipal and Industrial Wastewater Samples

John Welsh - OI Analytical

Industrial and municipal wastewater treatment plants must meet the strict demands required by National Pollution Discharge Elimination System (NPDES) permits for the discharge of treated wastewater. Operators and analysts require the capability to accurately determine TOC concentration over a wide dynamic range, as well as analytical instrumentation that is robust, easy-to-use, and provides a low cost of ownership.  This poster presents a performance study of a new combustion Total Organic Carbon (TOC) Analyzer which exceeds the requirements of the industry and regulators on a range of demanding effluent samples.