2022 Oral Presentations

The following abstracts had been received and accepted for presentation at the 2022 Gulf Coast Conference.

Abstract # 97 - Training Course
10/10/2022 - 8:00 AM - 5:00 PM - Ivy Room 2 - Moody Gardens Hotel

MONDAY SESSION * Diesel Fuel Test Methods - An Overview

David Forester - ASTM International

This 1-day course on test methods for diesel fuel has been especially developed for the Gulf Coast Conference. It draws some material from the regular 3-day ASTM Diesel Fuel Course, and adds specific details about manual and automated test methods that are used to evaluate batches of diesel fuel. Original test methods were manual procedures, and over the past few decades, instrument manufacturers have developed automated instruments to measure many properties.
Subjects to be discussed include:
  • ASTM D975, the diesel fuel specification used in the States;
  • Detailed properties and the relevant test methods;
Types of properties and test methods
  • Manual test methods versus automated test methods;
  • Relationships between various properties such as sulfur & lubricity / conductivity, gasoline contamination and flash point / viscosity; paraffin (wax) content and low temperature operability;
  • Additives used in diesel fuel and their impact on properties.
ASTM Standards Referenced
        Diesel fuel specification: D975
        Flash point: D93, D56, D3828, D7094
        Water & Sediment: 2709, D7619
        Distillation: D86, D2887, D7344, D7345
        Kinematic Viscosity: D445, D7042
        Ash: D482
        Sulfur: D5453, D7039, D129, D1266, D1552, D2622, D3120, D4294, D7220
        Copper Corrosion: D130
        Cetane Quality: D613; D4737, D976, D6890, D7668, D8183
        Aromatics: D1319, D976-80
        Low Temperature Operability: D2500, D5771, D5772, D5773, D4539, D6371, D7683, D7689
        Carbon Residue: D524
        Lubricity: D6079, D7688
        Conductivity: D2624, D4308


Diesel Fuels – An Overview

Abstract # 98 - Paper
10/11/2022 - 10:00 AM - 11:00 AM - Exhibit Hall A4

*KEYNOTE SPEAKER* Compact Analytical Instrumentation in the Petroleum and Petrochemical Industries: Portable Liquid Chromatography as an Emerging Technology

Dr. Milton Lee - Axcend, Provo, UT, and Brigham Young University, Provo, UT

A major trend in the analytical chemistry field today is to significantly reduce the size of analytical instrument components and products. Reduction in size generally allows greater mobility, simpler operation, lower cost, and greater productivity. These characteristics are especially important in the petroleum and petrochemical industries because of the broad-ranging needs for timely chemical measurements in some of the most diverse locations. Taking the instrument to the sample instead of the sample to an instrument that is permanently located in a laboratory makes much more sense in these industries compared to many others. Liquid chromatography (LC) has been slow to embrace compactness and portability compared to spectrophotometry and gas chromatography (GC), for example. Today, new developments in materials and hardware components have accelerated efforts to develop compact LC. In the last few years, truly portable gradient LC has become commercially available, offering small high-pressure pumping systems that can deliver microliter to nanoliter/min mobile phase flow rates, fittings and transfer lines that minimize dead volumes to preserve chromatographic performance, and multiple detector options including single wavelength on-column UV-absorption detection with LED light sources, multi-wavelength diode array detection (DAD), fluorescence detection and, of course, mass spectrometry (MS). Small diameter (< 0.3 mm i.d.) packed capillary columns can be pre-mounted in temperature-controlled, easy-to-connect cartridges that literally take less than a few minutes to install/exchange. Examples of applications that are particularly well suited for compact LC in the petroleum and petrochemical industries include point detection of hazardous chemicals in emissions and effluents, chemical process monitoring and optimization, purity assessment of reclaimed process water, determination of final compositions of petroleum products, measurement of additive levels in petroleum-derived fuels, and detection of fuel marker compounds. The extremely low mobile phase flow rates characteristic of portable/compact capillary LC minimize the cost and bother of purchasing and disposing of mobile phase solvents, and clearly position the technique in the elite class of “green analytical chemistry.”

Abstract # 99 - Paper
10/12/2022 - 1:00 PM - 2:00 PM - Exhibit Hall A4

*KEYNOTE* Activities of The NELAC Institute (TNI) to Improve Data Quality

Jerry Parr - The NELAC Institute

Part 1:  How a Quality Management System Improves Data Quality and Laboratory Performance Since its inception, individuals active in the US National Environmental Laboratory Accreditation Program (NELAP) have struggled to try and find information to convince others that implementing a Quality Management System (QMS) according to the requirements in the TNI Standard Management and Technical Requirements for Laboratories Performing Environmental Measurements improves data quality.  Over the years, various surveys and studies have been conducted to try and prove this assertion.  However, the problem has been, and always will be, we never know the true concentration of a contaminant in a sample.  All measurements are only estimates of the true concentration, and quality control data does not always directly correlate with the measurement of the actual contaminant. In 2019, TNI’s Advocacy Committee initiated a new effort to document improved laboratory performance and trust in the data provided by accredited laboratories.  This presentation will summarize the outcomes from the Committee’s efforts and provide real examples of why implementing a QMS based the TNI standard makes a real difference in both data quality and laboratory performance.

Part 2:  Evaluating the Goodness of Instrument Calibration for Chromatography Procedures Instrument calibrations in analysis methods using gas chromatography (GC) or liquid chromatography (LC) are usually created using either average response factor (RF) or linear (sometimes quadratic) regression equations. The quality, or “goodness,” of an Average RF calibration is measured by relative standard deviation (RSD) whereas the linear regression has historically been measured by correlation coefficient (r) or coefficient of determination (r2). This presentation will demonstrate that the goodness of a calibration measured by RSD is quite different than r/r2 and that while one is suitable as a calibration measure, the other is not. Relative standard error (RSE) is a way of extending the use of relative measures of calibration quality beyond the average RF calibration type.

Abstract # 100 - Training Course
10/13/2022 - 9:00 AM - 4:00 PM - Ivy Room 1 - Moody Gardens Hotel

THURSDAY CLASS * Complete Analytical Training for the Petroleum Chemist - Bridging the Gap Between Engineers and the Lab

Jean-Francois Borny - B.A.S.I.C.

This course will include a complete virtual tour of the analytical laboratory for the petroleum industry. We will discuss many analytical instruments and their basic function and technology. This will include GCs, ICP, ICP-MS, XRD, XRF, elemental analyzers, titrators and more. 

This course will also bridge the gap that some chemists experience while discussing the engineer needs including reading P&ID, block flow diagram, online analyzers, sampling, and sampling system. 

And finally, we will discuss the different standardized methodologies including ASTM, UOP, IFP, GPA methods and dive into QA/QC including repeatability and reproducibility. 

The course will be heavily supported by real world examples and as an open forum for questions and answers throughout the day.

The Fee for this course is $125.00 & includes lunch, please register at  Register To Attend and select Registration Type + Thursday Session from the drop down.

Abstract # 107 - Paper
10/11/2022 - 9:30 AM - 9:50 AM - Tulip

The comprehensive evaluation of Source Rock using Micro-Furnace Multi-Shot Pyrolysis GC/MS

Athena Nguyen - Frontier Lab Americas
Rojin Belganeh - Frontier Lab Americas

The increasing world population and the expanding world economy have precipitated a rush to find new sources of energy for developing new oil and gas sources. Exploration today often relies upon the geochemistry of the source rock from the play of interest. The importance of Rock Evaluation Pyrolysis and the presence of specific compounds or groups of compounds in source rock is of immense importance to industries engaged in assessing the potential of a given play. Although many laboratories continue to solvent extract the sample prior to analysis, others have found that thermal extraction of the source rock will often yield a faster more accurate determination of the organic content. In this presentation, the comprehensive evaluation of Source Rock was performed using micro-furnace Pyrolysis-GC/MS with eliminating the need for conventional sample preparation.

Abstract # 119 - Paper
10/12/2022 - 10:45 AM - 11:10 AM - Iris

Raman for Closed-Loop Process Control

Brian Rohrback - Infometrix, Inc.

 Much effort has been applied to put process spectrometers to work for a specified application:

  • Selecting instrument settings for best performance;
  • Automating method development for wavelength selection and preprocessing; and
  • Automating calibration updates.

At this point, there is only one task that remains for us to close the loop and completely automate the lifecycle of a Raman analyzer for any given purpose.  We need to identify when a calibration requires attention and then have a system in place to institute an adjustment without supervision.  Introducing a process Raman should be no more difficult to manage than installing a temperature sensor.

Abstract # 121 - Seminar
10/12/2022 - 10:55 AM - 11:25 AM - Bluebonnet

A New Gravimetric Dilution System for ICP and ICPMS Sample Preparation

Steve Twining - Elemental Scientific, Inc

ICP and ICPMS gravimetric sample preparation often requires the most skilled analysts performing high precision dilutions by weight, often in a hood, for hours on a daily basis.  Elemental Scientific has developed an automated technology that dilutes samples accurately and precisely.  This highly flexible system prepares a variety of samples over a wide viscosity range.  Combined with a second technology that incorporates non-mechanical gas infusion homogenization, automated crude oil gravimetric sample preparation is now possible.

Abstract # 122 - Paper
10/11/2022 - 9:10 AM - 9:40 AM - Rose

Rapid Determination of Refined Fuel Properties Using a Novel Solid State Raman Analyzer

Tom Dearing - MarqMetrix

Raman spectroscopy is an ideal candidate for refined fuels analysis, having the key attributes of specificity, sensitivity, speed and stability and simplicity.  In this paper, we will describe the methodology for collecting high quality Raman spectra and the strategy for turning the spectral data into information to inform the decision-making process.  Analysis of multiple fuel types including gasoline, jet and diesel as well as component streams such as reformate, isomerate and alkylate will be described as well as modeling strategies to ensure a simplified approach for laboratory workflow for technicians and operators.

Abstract # 123 - Paper
10/11/2022 - 8:30 AM - 8:50 AM - Floral Hall A2

Use of Thermo Scientific Trace GC for ASTM D2887B Accelerated Procedure with Alternative Carrier Gases

James Pachlhofer - Thermo Fisher Scientific

The world is experiencing yet another helium supply crisis.  ASTM International recognized this fact several years ago and requires that analytical methods up for renewal be tested using alternative gases by their ILS process so the alternative gases may be to be certified for use with the method. D2887B is the accelerated procedure method for this important simulated distillation method.  This accelerated procedure has been utilized for several years using helium carrier gas. Recently, an ILS was performed to certify hydrogen and nitrogen carrier gas together with helium to be acceptable carrier gases. Data will be presented and discussed using a Thermo Scientific Trace GC to demonstrate compliance to D2887B for the three carrier gases.  

Abstract # 124 - Paper
10/12/2022 - 8:30 AM - 8:50 AM - Floral Hall A2

A Fresh Approach to D5769 Analysis using a Thermo Scientific ISQ7610 Single Quadrupole GCMS

Amit Gujar - Thermo Fisher Scientific
Kenneth Free - Thermo Fisher Scientific
James Pachlhofer - Thermo Fisher Scientific

D5769 for Benzene, Toluene and Total Aromatics in Finished Gasoline by Gas Chromatography/Mass Spectrometry is the ‘gold’ standard method required for certification of gasoline in many countries and regions of the world.  The method challenges detection limits as well as linear ranges of the components of interest in GCMS.  Also, as changes in the composition of gasoline continue to evolve, this further challenges the GCMS instrumentation to comply with the method. The new Thermo Scientific ISQ7610 MS together with the new 1610 GC provides a fresh approach to overcoming these challenges.  The new Extended Dynamic Range Electron Multiplier used in the ISQ7610 provides the range necessary for the method without compromising any required MS hardware or operational parameters. Data will be presented and discussed demonstrating full compliance to the method using the Thermo Scientific GCMS.  All aspects of the method specifications including sensitivity, resolution, ion check tests, calibration, and reference material compliance tests will be presented.  In addition, the analysis of an ASTM D5769 ILS sample will be presented demonstrating excellent results.     

Abstract # 125 - Paper
10/12/2022 - 11:05 AM - 11:35 AM - Iris

MarqMetrix in the Middle: How to reduce cost and improve profit with Raman spectroscopy

Grant Kerkman - MarqMetrix

The financial health and wellbeing of Midstream Oil & Gas companies relies on minimizing cost and operational expenses without sacrificing quality or system reliability.  Limitations in analytical technology have prevented Midstream operators from fully unlocking their potential in cost reduction, until now.  By utilizing MarqMetrix’s revolutionary Raman spectroscopy, Midstream operators now can make crucial, data-driven decisions in real time to minimize costs and drive profitability.  This paper will outline the new capabilities brought to the Midstream market segment by the MarqMetrix All in One Raman analyzer by using innovative optics and chemometric modeling.  The paper will also provide guidance through three unique case studies: transmix reduction of refined fuels, LPG product blending, and terminal loading operations.  In all three cases, one will see that the speed of response and ability to perform quick, accurate measurement allows an operator to unleash the full potential of their operations.  By utilizing MarqMetrix’s novel Raman analyzer, a Midstream operator can decrease cost, boost profit, and maintain the same level of quality and reliability that the industry demands.  

Abstract # 127 - Paper
10/11/2022 - 2:10 PM - 2:35 PM - Tulip

Improved characterization of malodours from recycled plastics using TD–GC×GC–TOF MS

Matthew Edwards - SepSolve Analytical

The analysis of plastic has gained increased attention in recent years, due to the global push to move to a circular economy and use more recycled plastics, which require more rigorous quality control to ensure they will not produce harmful or odorous emissions.

However, there are several limitations with the existing methods for the detection of odours from plastics – such as, human sensory panels, eNose and GC-MS.

Here, we show how TD–GC×GC–TOF MS can address these challenges, by providing high sensitivity and improved separation of the odour profiles, prior to confident identification of the individual analytes.

Abstract # 132 - Seminar
10/11/2022 - 8:40 AM - 9:10 AM - Tulip

Recent developmewnts and Validation of a More Accurate Tool for Fuel Clarity by D8148, Spectroscopic Method for Haze in Fuels

Ranzy Morgan - Choice Analytical Inc.

Recent Developments and Validation of a more accurate tool for Fuel Clarity by D8148 Spectroscopic method for Haze in Fuels   Providing fuel with the necessary cleanliness has been desirable since the earliest days of motorized transportation. Engine manufacturers expend significant effort to protect sensitive components of modern high pressure fuel systems from fuel contaminants. With an unprecedented number of new fuel types and feedstocks entering the worlds fuel supply, the industry is becoming increasingly concerned about fuel cleanliness and clarity. Over the decades, engine manufacturers, fuel producers and fuel distributors, worked within ASTM to establish specification limits for fuel haziness and clarity. Because of the variability and subjectivity found with the current visible methods such as D4176 and because ASTM specifications may be applied anywhere within the fuel distribution systems, fuel pipelines and transport companies have traditionally not supported these efforts. During the last five years, major pipelines have worked closely to support the optics-based technology found in D8148. ASTM D8148 Haze Clarity index is an instrumental objective technique which eliminates the subjectivity of the visual haze methods. D8148 measures and reports haze results in two formats 1) Instrumental Haze Rating (IHR) ranging from 1-6 which is calibrated to be equivalent to the D4176 Visual Haze rating, and 2) Haze Clarity Index (HCI) ranging from 50-100.  HCI provides greater resolution and specificity of fuel cleanliness.  With the large amount of data provided in the recent D8148 Interlaboratory Study, as well as CRC report 675, which compares D8148 to D4176 and actual amounts of water in fuel samples, it may be the time to seriously reconsider putting measurable limits around fuel cleanliness. This presentation will review the D8148 method, recent ILS results along with the data and conclusions presented in CRC report number 675.

Abstract # 133 - Paper
10/12/2022 - 12:30 PM - 12:55 PM - Iris

In-line Naphtha Property Monitoring via Raman Spectroscopy

Giancarlo Aguirre - Process Instruments, Inc.
Lee Smith - Process Instruments, Inc.

The use of Raman spectroscopy for analysis of the various refinery products has increased dramatically in the last 20 years.  While ASTM Laboratory tests are still needed and are the gold standard in order to build such models, the need to constantly run them is less. This advantage can be expanded to the online monitoring of products such as Naphtha where this fraction is a key component of the gasoline blending process and/or feed of other units within the refinery.   Naphtha can be consistently separated into two fractions, light and heavy.  Ranging from C5/C7 for the light cut and up to C9 for heavy. Regardless of the Naphtha process, Raman spectroscopy can be an important tool to verify the unit targets and provide tight control off key properties.  It is also used extensively for distillates such as Jet and Diesel.   Throughout this presentation examples will be shown of the analysis Raman can be implemented for, with the aid of regression and classification type models along with corresponding laboratory test data. Examples of the instrumentation used in refinery settings along with feedback from active users will also be provided.   Raman has allowed unit operators to monitor and control their blends more effectively without having to invest in multiple individual property analyzers.  

Abstract # 134 - Seminar
10/12/2022 - 10:05 AM - 10:50 AM - Floral Hall A2

Optimizing Process Operations with On-Line Process Monitoring

Kirk Chassaniol - Thermo Fisher Scientific

Industrial processes have common needs: reliable, accurate, and timely methods for analyzing process chemistry. Continuous monitoring with on-line liquid chromatography (LC) lets you detect process variations earlier than laboratory-based measurement and long before yield is impacted or costly process shutdowns become necessary. By improving process monitoring capabilities, you can fine-tune the process chemistry to maximize efficiency and reduce operating costs. Thermo Scientific™ Dionex™ Integral™ systems provide cost-effective, flexible solutions to apply on-line ion chromatography (IC) or high performance liquid chromatography (HPLC) to applications in a controlled setting, such as a laboratory or in a more challenging industrial environment. System modularity allows for the addition of modules and enclosures to tailor a configuration to meet specific needs. Several examples of how such systems have been applied to monitor waste and process streams will be presented.

Abstract # 135 - Seminar
10/11/2022 - 9:00 AM - 9:45 AM - Floral Hall A2

How discrete analyzer is bringing automated simultaneous multiparameter testing for process water and wastewater analysis

Kirk Chassaniol - Thermo Fisher Scientific

Traditional wet chemistry techniques have been used for years to undertake nutrient analysis of process water, wastewater, and soil samples. However, these approaches are slow, labor-intensive, involving hazardous reagents that add substantial costs for waste disposal.  This presentation will discuss the use of automated discrete analyzers and the associated regulatory-compliant system methods for the determination of nutrient levels, pH, and conductivity in routine water analysis.  Participants will also learn that the integrated discrete analyzers can help laboratories consolidate multiparameter tests onto one automation platform and enable a faster, safer, and easier workflow for productivity improvement and cost reduction. 

Abstract # 136 - Seminar
10/11/2022 - 12:00 PM - 1:00 PM - Floral Hall A2

Chromeleon Chromatography Data System Tips and Tricks.

Larry West - Thermo Fisher Scientific

In this session we will have a live session showing special topics of interest; which includes integration, reporting, data imports and exporting special parameters to third party software packages (i.e. LIMs, etc.). We will cover all Chromeleon Versions and Atlas. 

We highly desire audience participation with questions and topics on the day of presentation.

Abstract # 137 - Seminar
10/12/2022 - 11:20 AM - 11:50 AM - Floral Hall A2

Smarter, not harder: Chromeleon CDS and GC SMART Syringes for petrochemical separations

Larry West - Thermo Fisher Scientific

The petrochemical industry faces many challenges with chromatography that can cause frustration, instrument downtime, and significant costs. The Thermo Scientific™ Chromeleon™ Chromatography Data System (CDS) has built-in feature sets that can help overcome these challenges. During this session, we will discuss three of these features:   1- The use of report triggers that can isolate failed actions 2- The use of email notifications for early warning of failed actions and 3- How Thermo Scientific™ GC SMART Syringes communicate with Chromeleon CDS to improve uptime and performance     Each of these features can mitigate challenges, but in combination can make a huge impact.

Abstract # 138 - Seminar
10/12/2022 - 8:50 AM - 9:50 AM - Floral Hall A2

Best Practices for the analyses of complex samples by ICP-OES and ICP-MS: Streamline workflow for accurate results

Mike Mourgas - Thermo Fisher Scientific
Sabrina Antonio - Thermo Fisher Scientific

Trace and ultra-trace analyses of elemental constituents and contaminants in environmental and industrial samples led to the demand for sensitive multi-element techniques such as ICP-OES and ICP-MS. Innovations in instrumentation enhanced robustness, performance, and productivity. However, achieving accurate results remains a challenge, especially for complex samples containing suspended and dissolved solids, organic compounds, salts, etc. Systematic errors during preparations, physical interferences from matrix components, and spectral interferences contribute to the challenges. 

In this presentation, recommended best practices for the elemental analysis workflow from sample preparation to analysis will be discussed.  Learn how streamlining processes within the workflow save time, resources, and help to achieve accurate results and quality data. 

Abstract # 139 - Seminar
10/12/2022 - 11:50 AM - 12:50 PM - Floral Hall A2

Thermo Scientific Qtegra Software Demonstration: Intuitive and Easy Method Development for ICP-OES and ICP-MS

Mike Mourgas - Thermo Fisher Scientific
Sabrina Antonio - Thermo Fisher Scientific

Have a closer look at the intuitive, streamline workflow platform of the Thermo Scientific Qtegra Intelligent Scientific Data Solution (ISDS) software for ICP-OES and ICP-MS analyses with a live demonstration on method development, optimizing parameters, data review, and report generation. Also, learn about the software features that simplify the correction of advanced spectral interferences. 

Abstract # 140 - Paper
10/12/2022 - 10:50 AM - 11:20 AM - Floral Hall A2

How clumped isotope analyses drive a deeper understanding of petrochemical processes

Darren Tollstrup - Thermo Fisher Scientific
Nina Albrecht - Thermo Fisher Scientific

Classical stable gas isotopes, such as δD, δ13C, and δ18O, are well-established and valuable tools in various fields of earth sciences. They aid in constraining genetic mechanisms, provenance, transport processes, and formation temperatures. Their geothermometric usability is however limited as they lack an absolute temperature dependency. Clumped isotope geochemistry overcomes this limitation since the equilibrium distribution (‘clumping’) of heavy isotopes within multiply substituted molecules is solely dependent on the formation temperature.

The most investigated clumped isotope systems are clumping in CO2 and in CH4. It has been demonstrated that the associated thermometry delivers highly precise carbonate and methane formation temperatures. When two clumped isotopologues of one species are analyzed, it is even possible to pin down kinetic biases in cases where a sample is deviating from the expected thermodynamic equilibrium. Apart from geothermometry and the identification of kinetic processes, the addition of clumped isotope signatures to the classical stable isotope geochemist’s toolbox enables a refined forensic source apportionment of natural samples.

In this presentation we will illustrate the analytical setup (IRMS and HR-IRMS) to perform the above-mentioned measurements, and we will focus on how clumped isotopes add fresh insights into petroleum research. Besides CO2 and CH4, we will also give a perspective on the potential of clumped isotope analyses in N2, and H2, as typical compounds in natural gas reservoirs.

Abstract # 141 - Paper
10/11/2022 - 8:00 AM - 8:20 AM - Iris

Evaluate House Deionized(DI) Water with ICP-OES and ICP-MS

Eric Tang - Lummus Technology
Jean-Francois Borny - Lummus Technology

Deionized (DI) water is frequently used in our lab and pilot plant. In fact, large quantity of DI water is consumed daily.  To reduce the cost, a DI unit was installed onsite.  It is necessary to monitor the quality of DI water.  DI water produced from our house DI unit is analyzed  with ICP-OES and ICP-MS. Data are evaluated in comparison with that of both  commercial ASTM I and ASTM II water. Detailed information will be provided.

Abstract # 142 - Training Course
10/12/2022 - 2:30 PM - 3:30 PM - Iris

Unraveling the power of X-Ray Fluorescence technique for accurate quantitative analysis of Industrial materials

Poulami Dutta - Dow Chemical

X-ray Fluorescence (XRF) is an immensely powerful analytical technique for inorganic elemental analysis and is widely used in industry for different quantitative analysis needs including catalyst supports, promoters, polymer additives. Different categories of XRF instruments include high-end wavelength dispersive (WD) floor models to simple but rugged energy dispersive (ED) bench-top units. With recent advances in instrumentation and affordability, it is now possible to implement robust, accurate and precise EDXRF quantification methods in manufacturing laboratories that would traditionally require use of WD instruments available at a R&D lab only allowing on-site data acquisition for process control. It is also possible to use simple ED units to extract location-specific elemental distribution using benchtop Micro XRF instruments. Aside from instrumentation, sample preparation is critical for achieving high quality XRF data and accurate quantification. This workshop would be focused on highlighting different XRF technologies and sample preparation tools, highlighting practical examples of solving real life challenges.

Abstract # 143 - Seminar
10/11/2022 - 1:20 PM - 1:50 PM - Iris

To be or Not to be -- nuances in laboratory QA/QC compliance with accreditation requirements

Harold Longbaugh - City of Houston, DWO

Chemistry Laboratories have various accreditations (ISO-9001, ISO 17025, NELAC, etc.). In order to maintain those accreditations, they have to go through audits from the accreditation issuing bodies at pre-determined frequencies, and satisfy all the conforming requirements. By utilizing a few anonymous actual situations/cases in past TNI (the NELAC Institute) audits into a game-show type of interactive format, to foster discussions among laboratory professionals and auditors/assessors of the compliance strategies and nuances to reduce the number of non-conformance findings during future audits, hoping to benefit all participants by comparing accreditation requirements and auditor expectations.

Abstract # 144 - Paper
10/11/2022 - 1:50 PM - 3:20 PM - Hibiscus

Omnic Software Tutorial for IR/Raman Spectroscopy

Cam Macisaac - ThermoFisher Scientific

This workshop will cover Omnic software, the popular platform for running Thermo Fisher FT-IR, FT-NIR, and Raman spectrometers. A live software demonstration will be given to highlight features of Omnic, which will include collection of data from a working spectrometer. A live demonstration of TQ software will be given illustrating FTIR, FT-NIR and Raman quantitative and qualitative methods. Suggestions will be given on how to diagnose chemometric methods to ensure they accurately predict. Some pitfalls will be covered to avoid improperly modeled methods.  In addition, an overview of Macros/Basic automated workflow software will be given. This software is designed to build pre-program quantitative predictions. The Macros language can also automate many other software functions, like basic kinetic routines.

Abstract # 147 - Seminar
10/12/2022 - 11:25 AM - 11:55 AM - Bluebonnet

Moving beyond D445 with the simplicity of D7042

Tobias Fleiss - Anton Paar GmbH

How to transition from D445 to D7042 and considerations when using the new standard. How to run samples with ASTM method D7042 while saving time, money, lab space and much more.

Abstract # 148 - Paper
10/11/2022 - 9:20 AM - 9:40 AM - Iris

Viscosity: Not all measurements are created equal: Shear rate, shear stress, shear range- oh my.

Irene Pena - Lummus Technology

Most simple viscometers provide information at a single point whereas rheometers examine behaviors of the fluid over a range of points producing a flow curve. Rheological measurements are by definition far more complex than kinematic or rotational viscometer measurements because they evaluate flow properties such as shear thinning, shear thickening, viscoelasticity, and even structural recovery. When we evaluate properties of this nature, even one’s technique will affect results.

This presentation will take a closer look at how varying techniques affect rheological measurements.

Abstract # 149 - Paper
10/12/2022 - 9:40 AM - 10:05 AM - Tulip

“FIDIG” - FID Ignition Guaranteed

Matthew Monagle - Advanced Industrial Chemistry Corp.

It has been the author’s experience, over many years, that the automated process of lighting an FID is often unsuccessful.  In this situation, it is necessary to invoke a process affectionately known by the author as “Puff the Magic Dragon” to get the detector to ignite.  FIDIG solves this problem.  A simple modification to an FID chimney results in consistent repeatable FID ignition.  Implementing FIDIG means that an FID will ignite without external assistance.  It also means the detector can be turned off when not in use and save significant amounts of air, hydrogen and make-up gas. 

Abstract # 151 - Workshop
10/11/2022 - 12:00 PM - 12:45 PM - Rose

Precise Back Titration Method for Determination of Bromine Number

Tore Fossum - Tor Systems
Alan Cummings - Lummus Technology

Unsatisfactory repeatability and reproducibility of bromine number by ASTM D1159 and bromine index D2710 prompted the investigation of an alternate method that would deliver more precise and accurate results.  The precision of a classical titration is due to being able to determine the equivalence point exactly.  However, bromine number is not an equivalence point titration.  It is instead a titration to a diminished rate of bromine uptake.  Measuring this rate is dependent on the voltametric or amperometric detection of the apparatus, on the rate of delivery of titrant, the geometry of the detecting electrodes, and on the reactivity of the sample to free bromine.  Finding the bromine number reliably is a challenge in one lab with one instrument, but getting uniform results with various manufacturer's instruments in different labs has been difficult.  Therefor we propose a method where the bromine reagent is added at one time in excess, allowed to react with the olefin, and the remaining bromine titrated using a classical redox equivalence endpoint.  A blank of the same amount of bromine is compared to the remaining bromine to give the bromine number.  The endpoint is a standard equivalence redox inflection which should be reliably detected no matter which lab or which manufacturer's instrument is used.  We present results with a variety of hydrocarbon samples and standards by the classical D1159 compared to the back titration method.  A discussion will follow, with plans for an ILS at the next ASTM D02 meeting in December.  Potential participants are invited to attend. 

Abstract # 152 - Seminar
10/11/2022 - 12:30 PM - 1:05 PM - Wisteria

LUMAâ„¢: New Vacuum Ultraviolet Gas Chromatography for Low Level Detection of ACCUTRACEâ„¢ Fuel Markers

Marla Gilbert - The Dow Chemical Company
James Griffith - The Dow Chemical Company
Stephanie Perez - Kelly Services
JC Reyes - The Dow Chemical Company
Jeff Johnson - The Dow Chemical Company
Brian Jazdzewski - The Dow Chemical Company

The LUMA™ is a new smaller footprint gas chromatography detector developed by VUV Analytics.  The detector measures from 120 to 500 nm, inclusive of the vacuum ultraviolet spectrum range from 120 to 240 nm, nd collects up to 4 or 12 wavelength bands simultaneously depending on configuration. The LUMA™ is capable of collecting data with a chromatography data system to generate a chromatogram for peak detection.  As a proof of concept, the LUMA™ is being tested for several applications within Dow®, one of which is for detection of fuel markers.  Fuel markers are utilized globally to protect against fuel theft and laundering.  This seminar will highlight the features of the LUMA™ detector and possible application in fuel marker analysis with a single dimension gas chromatography method, as well as a two-dimensional gas chromatography method with heart-cutting by dean’s switch.

Abstract # 154 - Paper
10/12/2022 - 10:45 AM - 11:05 AM - Tulip

ASTM D8351-22: The newly approved Standard Test Method for Determination of Trace Elements in Biodiesel and Biodiesel Blends by Microwave Plasma Atomic Emission Spectrometry (MP-AES)

Jenny Nelson - Agilent
Paul Krampitz - Agilent

This talk will cover the new ASTM Standard Test Method for Determining Trace Elements in Biodiesel and Biodiesel Blends by Microwave Plasma Atomic Emission Spectrometry (MP-AES). This test method covers determining elements in biodiesel and biodiesel blends by MP-AES; calcium (Ca), magnesium (Mg), phosphorus (P), potassium (K), and sodium (Na). It is well understood that the presence of metals and metalloids in engine fuels can influence the performance of engines and contribute to shortening the lifetime of the equipment. In addition, some elements act as catalyst poison contributing to increases in the number of unwanted gases and particulate matter emitted by vehicles.This talk will cover the new ASTM Standard Test Method for Determining Trace Elements in Biodiesel and Biodiesel Blends by Microwave Plasma Atomic Emission Spectrometry (MP-AES). This test method covers determining elements in biodiesel and biodiesel blends by MP-AES; calcium (Ca), magnesium (Mg), phosphorus (P), potassium (K), and sodium (Na). It is well understood that the presence of metals and metalloids in engine fuels can influence the performance of engines and contribute to shortening the lifetime of the equipment. In addition, some elements act as catalyst poison contributing to increases in the number of unwanted gases and particulate matter emitted by vehicles.

Abstract # 157 - Paper
10/12/2022 - 2:00 PM - 2:30 PM - Iris

Fast and Reliable Chloride Monitoring in Refinery Processes by EDXRF

Daniel Pecard - Bruker AXS LLC

In this presentation, we will share details about the instrument calibration, measurement conditions and sample throughput using a X-Ray Fluorescence (XRF) spectrometer (S2 POLAR) for Chloride analysis. Analytical data, reproducibility data and lower limits of detection, will be presented, including real crude oil measurement.  An outlook and overview of what other refinery applications that can be covered with the same instrumentation will be provided as well.

Abstract # 158 - Paper
10/12/2022 - 9:15 AM - 10:05 AM - Hibiscus

Recent Advances in FTIR Gas Analysis

Kelly McPartland - Thermo Fisher Scientific

Newly developed Optically Enhanced FTIR (OE-FTIR) technologies are lowering system sensitivities to levels never previously achieved by FTIR, parts-per-trillion measurements for certain applications.  With the added sensitivity, detection limits for many applications are no longer dependent on the detector noise, but rather the spectral interferences.  New technologies are also being deployed to eliminate or reduce this “spectral interference noise” by collecting pseudo-calibration data during sample data collection. The OE-FTIR and the spectral interference removal technology, along with process and environmental applications, will be presented.

Abstract # 159 - Paper
10/12/2022 - 10:50 AM - 11:40 AM - Hibiscus

Solutions for Ethylene Oxide Source Emissions Monitoring

Kelly McPartland - Thermo Fisher Scientific

The measurement of Ethylene Oxide (EO) from stationary sources has recently gained significant interest due to new proposed emission and exposure standards. To measure any gas at ppb levels in real-time requires ultra-sensitive instrumentation and insensitivity to cross-interferences present in the sample matrix. Sample transport can also be a challenge at these levels, and adequate QA/QC must be performed to demonstrate that the technology is producing accurate and defensible results. All these challenges will be discussed and how they are handled within FTIR-based continuous emissions monitoring (CEM) systems.

Abstract # 160 - Paper
10/11/2022 - 1:00 PM - 1:50 PM - Hibiscus

Polymer Grade Ethylene and Propylene Process Monitoring by Optically Enhanced FTIR

Kelly McPartland - Thermo Fisher Scientific

Mid-infrared FTIR gas analyzers have the unique ability to monitor many compounds over a wide dynamic range, which allows for the simultaneous measurement of % to trace level impurities without physical separation. Historically, these FTIR gas analyzers were only capable of measuring in the mid-ppb range. However, new advances in FTIR gas analysis now allow for impurity measurements at single digit ppb levels, which rivals the sensitivity of GC-based techniques, but with faster analysis times and lower cost of ownership. This presentation will discuss new hardware advances along with data demonstrating the measurement of impurities in bulk ethylene and propylene.

Abstract # 163 - Seminar
10/11/2022 - 12:00 PM - 1:00 PM - Hibiscus

Theory and Applications of Fourier Transform Infrared Spectroscopy and the Handling of Samples

Andrew Schmitz - ThermoFisher

Infrared (IR) spectroscopy is a quick, reliable, non-destructive technique that takes advantage of molecular vibrations to identify and study chemicals. Fourier Transform Infrared (FTIR) spectroscopy is the main method in executing IR spectroscopy. With IR spectroscopy a user can identify compounds, functional groups in organic molecules, interaction between a molecule and its local environment, and perform quantitative analysis such as concentration measurements just to name a few. There are several techniques in FTIR spectroscopy such as drifts, attenuated total reflectance and transmission. This presentation will cover the theory of FTIR spectroscopy along with the different sampling techniques and their applications.

Abstract # 164 - Seminar
10/11/2022 - 9:00 AM - 9:50 AM - Hibiscus

Microspectroscopic Sampling – FTIR and Raman Microscopy

Andrew Schmitz - ThermoFisher

Fourier Transform Infrared (FTIR) and Raman spectroscopy both utilize molecular vibrations to study and analyze chemicals The former uses absorption spectroscopy where the latter involves light scattering off the molecule. The two techniques are used in microspectroscopy for material >100 µm in size. This presentation will illustrate the applications and advantages of both techniques depending on the type of sample being studied.

Abstract # 165 - Paper
10/12/2022 - 10:05 AM - 10:50 AM - Hibiscus

Near Infrared for Process Control

Cam MacIsaac - ThermoFisher Scientific

Implementation of Fourier Transform Near Infrared Spectroscopy (FT-NIR) can be used to successfully replace the need for costly chemical titration methods in the lab, while also improving repeatability of compositional measurements in a sample.  FT-NIR is widely used in analyzing solid and liquid samples to characterize the quality and quantity of various components of the sample. At line and in-line applications allow for taking lab analysis directly to the sampling point in production, reducing sample timing and improving manufacturing efficiency. Real-time data analytics and robust chemometrics yield greater insight into sample characteristics and allow for continuous monitoring for any changes in the manufacturing process. This talk will cover the fundamentals of FT-NIR technology, highlight some common applications of taking the technology from lab to line, as well as how to successfully apply chemometrics to obtain the most information from your samples.

Abstract # 169 - Paper
10/11/2022 - 12:45 PM - 1:15 PM - Rose

AI Chemometrics: Automation for the Development, Validation, and Maintenance Processes for Predictive Process Analytical Measurement Systems

Paul Giammatteo - 4IR Solutions, Ltd
Dror Albo - 4IR Solutions, Ltd

Application of Chemometrics from initial feasibility to validated on-line predictive measurements is labor and data intensive.  Specifically, multiparameter model development and maintenance procedures are data intensive processes arising from process and stream variations, production changes, and/or regulatory requirements.

Utilizing AI algorithms significantly reduces labor intensive steps in Chemometrics.  Applicable to a variety of analyzer systems, this presentation highlights AI “automation” for model building, prediction validation, performance verification, and reporting.  Rigorous integration with a variety of LIMS and DCS/Plant Control Platforms, coupled with intuitive graphical interfaces and reporting, facilitate effective Chemometric utilization and support over a range of skill levels.

Abstract # 170 - Paper
10/12/2022 - 9:55 AM - 10:25 AM - Iris

Real-Time Measurement of Impurities in Ethylene Production

Koji Ishikawa - HORIBA Instruments Inc
Brian Ross - HORIBA Instruments Inc

HORIBA has developed a new Process Laser Gas Analyzer (PLGA) using a unique technology called IRLAM with Quantum Cascade laser (QCL) as the light source. The QCL’s and IRLAM algorithms are optimized for each application.  The analyzer houses up to six lasers in one enclosure for dedicated application. For Ethylene production it exhibits high sensitivity for Acetylene (C2H2), Carbon Monoxide (CO) and Carbon Dioxide (CO2) measurements. Field trials were conducted over six months to determine the performance of the analyzer when compared with general QCL analyzer and gas chromatographs (GC) measuring the same hydrocarbon. The analyzer achieved high stability performance for each laser and was able to rapid detect any upset condition. The PLGA-1000, with IRLAM, performs this critical C2H2 measurement both at the C2 Splitter and the Acetylene converter locations.

Abstract # 171 - Paper
10/11/2022 - 1:50 PM - 2:15 PM - Iris

Quality Control Implementation: Systems vs Parts

Jean-Francois Borny - Lummus Technology

Paraphrasing Peter Drucker’s famous quote, there is a difference between doing things right and doing the right things. The first refers to leadership, the second refers to management. When it comes to quality control, there is a tendency to strive for continuous improvement, the idea being if problems are addressed one at a time, the overall quality will improve. But getting rid of what does not work does not necessarily produce the desired results. So, the question is; Are we doing things right or are we doing the right things?

This presentation will propose a Statistical Quality Control approach that looks at the analytical laboratory as a whole system rather than individual parts and how to refine the system to achieve the desired quality improvements. The performance of a system depends on how the parts fit, not how they perform separately. We have plenty of knowledge, let’s increase our wisdom. Let’s explore quality and continue our journey from efficiency to value.

Abstract # 172 - Paper
10/11/2022 - 12:40 PM - 1:20 PM - Iris

Biodiesel Sulfur Test Method Comparison, Renewable Diesel vs. Biodiesel, and the Importance of Oxygen Correction for XRF

Leslie McHenry - XOS

Although ASTM D5453 (sulfur by UVF) is the referee sulfur method according to the D6751 biodiesel specification, D7039 (sulfur by MWDXRF) may also be used.  During this webinar, data from the ASTM Biodiesel Proficiency Testing Program will be examined to see how the two sulfur methods compare.  Also discussed is the importance of compensating for oxygen in biofuels when measuring sulfur by XRF and its impact on measurement results if not properly compensated for.  Lastly this webinar will review two common methods of oxygen compensation, and what this means when measuring sulfur in diesel, biodiesel, feedstocks, and renewable diesel by XRF.

Abstract # 173 - Paper
10/11/2022 - 8:00 AM - 8:30 AM - Wisteria

Analysis of Recycled Plastics using the VUV Analyzerâ„¢ for Alternative Feedstocks

Alex Hodgson - VUV Analytics

Plastic waste is recognized as a significant environmental challenge as well as an opportunity. Many organizations are actively involved in recycling plastic waste and by using pyrolysis technologies converting it into usable petrochemical feedstocks. The output of this process is challenging to analyze with traditional analytical approaches used for traditional hydrocarbon streams. This presentation will preview a new automated application using Gas Chromatography (GC)-Vacuum Ultraviolet Spectrometry (VUV) that provides accurate identification and PIONA-type quantification of pyrolysis oils over a broad carbon number range.

Abstract # 174 - Paper
10/12/2022 - 10:30 AM - 10:55 AM - Bluebonnet

Comparison of Sulfur Chemiluminescence Detectors (SCD): Four models, three vendors

Alan Cummings - Lummus Technology

SCD’s are the “go to” for sulfur speciation since the mid 1990’s.  Other sulfur detectors preceded them for sulfur speciation but had their own challenges.  SCD’s address these challenges with superior linearity, equimolarity and detection limit with minimal matrix interferences.  Because of SCD’s benefits, there are now three vendors with their own SCD on the market.  

Lummus Technology has all three vendor SCD’s and 4 different models.  This presentation will focus of comparing these four detectors, with the same sample sets and assess which one is more reliable, more stable and has better stability, including an insight of the reason these detectors behave as presented.

Abstract # 175 - Paper
10/11/2022 - 8:00 AM - 8:30 AM - Bluebonnet

Advanced Hydrofluorocarbon Leak Detection using Optical Gas Imaging Cameras

Craig O'Neill - Teledyne FLIR
Ryan Cochran - Chemours

Optical gas imaging (OGI) cameras have been used by a variety of industries for many years since the inception of the technology in 2005.  Most notably in the oil and gas industry for the detection of hydrocarbon gases.  More recently, the petrochemical industry has looked to adopt new technologies like OGI for effective leak detection of hydrofluorocarbon gases.  Historically, leak detection was performed with either handheld instruments, like a toxic vapor analyzer, or fixed ambient air monitoring solution where a technician would be deployed to find a leak source after an alarm.  Optical gas imaging cameras allow operators to streamline the leak detection and repair (LDAR) process by finding leaking sources faster and from greater distances than before, increasing operational safety. 

Abstract # 176 - User Group
10/11/2022 - 3:00 PM - 3:20 PM - Rose

Fenceline Monitoring Solutions for Industrial Facilities with SIFT-MS. Fixed Installation and Mobile Deployment

Paul Johnson - Syft Technologies
Leslie Silva - Syft Technologies

SIFT-MS is a real-time field-deployable mass spectrometer that provides online trace analysis of ambient air with detection limits down to sub-ppbv levels.  SIFT-MS has some key characteristics that make it ideally suited to industrial fence-line monitoring applications:

-SIFT-MS can be installed at the fenceline for direct point-source air quality measurements providing a 24/7 data stream with automated instrument validation with minimal periodic operator intervention.

-SIFT-MS provides highly sensitive monitoring of a diverse range of species through the utilization of both positive and negative chemical ionization agents.  Target compounds include: acid gases (incl. HCl, HF),  permanent gases (incl. CO2, SOx, NOx, Ozone), volatile organometallics, oxygenates (incl. aldehydes; formaldehyde), nitrogen-containing compounds (incl. amines; ammonia), reduced sulfur compounds (incl. hydrogen sulfide), halogenated compounds, and hydrocarbons.

-In addition to the mass spectral identification of species, SIFT-MS provides an additional dimension of chemical selectivity through the simultaneous application of multiple reagent ions.  This vastly reduces the number of false-positive reports compared with online mass spectrometers that rely on a single ionization mechanism.

Several case studies will be presented, including the deployment of SIFT-MS for 24/7 continuous monitoring at fixed installations and mobile measurements at the fenceline of a Korean semiconductor manufacturing facility (Samsung Electronics), and the localization of fugitive emissions at a gas refinery in New Zealand. Highlights from the Syft Clean Air Roadshow in 2021 will also be discussed.

Abstract # 177 - Paper
10/11/2022 - 8:30 AM - 8:55 AM - Wisteria

The GC-VUV Analyzerâ„¢ Platform

Dan Wispinski - VUV Analytics

Gas chromatography vacuum ultraviolet (GC-VUV) spectroscopy has gained wide-spread use.  The adoption of GC-VUV is due to acceptance by voluntary consensus standards boards (VCSBs), its flexibility and versatility, recognition by regulatory bodies and the adaptability to complex R&D functionality.    The VUV Analyzer™ integrates four VCSB methods (ASTM D8071, ASTM D8267, ASTM D8368 & prEN17734) into one platform, providing an automated, fast and accurate approach for gasoline, jet fuel, and diesel analysis.  A broad range of conventional, non-conventional and renewable fuels are included.  The platform was developed to seamlessly switch between four VCSB methods using the same hardware and software.  This paper will describe the latest ASTM and CEN developments for these four methods and how they integrate into one automated system - the VUV Analyzer™ platform.

Abstract # 178 - Paper
10/11/2022 - 8:55 AM - 9:25 AM - Wisteria

Refinery Modeling and Process Performance Improvement using Verified Hydrocarbon Analysisâ„¢

Dan Wispinski - VUV Analytics
Peter Spitz - AmSpec LLC

Improving process unit performance requires a cyclic approach to sampling, measuring, controlling, and ultimately managing value.  Model predictions rely on precise measurements.  The characterization of naphtha feed to the reformer enables mathematical models to predict yields, catalyst life and final product quality.  The naphthene and aromatic content of the feed (N+A) is a critical input parameter.  This paper will provide insights into the (N+A) measurement process.  Naphtha proficiency test program data indicating multi-laboratory precision for traditional techniques will be discussed.  This data indicates current best industry practice and precision.  ASTM D8369 using Verified Hydrocarbon Analysis™ (VHA) Appendix X3 parameters (ambient initial oven temperature and hydrogen carrier) as applied to naphtha feed and reformer product is also presented. 

Abstract # 179 - Paper
10/11/2022 - 2:00 PM - 3:00 PM - Rose

Save Time and Reduce Maintenance Expense in Viscosity Testing

Lupe Balboa - PAC LP

Reducing test measurement time and instrument maintenance expense are everyday concerns for lab managers and operators. Using the approved ASTM D7945 method, the new Phase Technology/PAC OptiMVD provides quick, easy, automatic viscosity and density measurement for lubricant oils, base stock, and distillate fuels. Learn more about how the OptiMVD solves current D445 challenges facing lube/additive producers, blenders, refineries and third-party labs today. The OptiMVD was awarded new product of the year at GCC in 2021.

Abstract # 180 - Paper
10/12/2022 - 8:30 AM - 9:00 AM - Bluebonnet

Reduced Sample Volumes to Increase Sample Throughput for US EPA Method 1664B

Michael Ebitson - Biotage

Removal of oil and grease from wastewater is imperative as it can negatively affect human health and drastically reduce the diameter of sewage pipes, restricting flow of wastewater and causing backups.  Due to the nature of some samples potentially exceeding the limit of 1000 mg/L of oil and grease, US EPA Method 1664B has allowed for the reduction of sample volumes for gravimetric analysis.   With this study, labs are no longer bottlenecked with samples that are heavily laden with oil and grease and are challenging to extract.  The reduction of sample volumes in turn reduces the amount of oil and grease that needs to be filtered out from any given water sample that was originally one liter in volume, decreasing the sample loading time and increasing sample throughput.  The extraction process is further streamlined using two different types of automated extraction systems.  The data from 250 mL sample extractions demonstrates that the recovery of oil and grease on each extraction system, is within the necessary recovery range outlined in US EPA Method 1664B, remaining compliant with the quality and consistency requirements.  The difficulty of extracting 100 mL samples will also be discussed.

Abstract # 181 - Paper
10/12/2022 - 8:00 AM - 8:30 AM - Bluebonnet

Breaking Through the EPH Fractionation Bottleneck with Automation and Multiple Cartridge Formats.

Michael Ebitson - Biotage

In today’s environmental laboratories there are many methods and techniques being used in sample preparation. One technique-driven method that has been described as a bottleneck is the fractionation of Extractable Petroleum Hydrocarbons (EPH) in water and soil extracts. This method recommends using 5g, 20 mL silica gel cartridges to separate the aliphatic and aromatic compounds from the sample extract to be analyzed by GC-FID.

  As laboratory challenges grow with increased samples loads, turnover of personnel while taking in highly concentrated water and soil matrices for extraction, it can be challenging to streamline the fractionation workflow. With such hurdles it often results in having to refractionate the sample and or entire batch, creating a bottleneck in sample throughput.  

This work will demonstrate the advantages and disadvantages of EPH cartridges in multiple formats and fractionation platforms. This work will highlight how the workflows can help laboratories overcome this bottleneck with consistency and quality by utilizing batch type processing with automation while demonstrating how cross-contamination is eliminated.

Abstract # 182 - Paper
10/12/2022 - 9:05 AM - 9:25 AM - Wisteria

Techniques for Microstructure Characterization of Functionalized Ethylene/Propylene Polyolefins

Anthony Gies - Dow Chemical

A combination of matrix-assisted laser desorption/ionization mass spectrometry (MALDI-MS), collision-induced dissociation (CID), nuclear magnetic resonance (NMR), and size exclusion chromatography were used to examine the end-group and architectural distributions within a model but-3-en-1-yl(phenyl)phosphine (BPP) functionalized poly(ethylene-co-propylene) (EP), which had been synthesized using a dual-headed chain shuttling agent (DHCSA). This study will highlight several interesting findings: (i) CID fragmentation results were used to build general fragmentation models; (ii) these models provided insight into the EP polymer chemical connectivity, end-groups, and incorporation of the DHCSA; and (iii) lastly, these results will be used to explain the observed EP polymer distributions.

Abstract # 183 - Paper
10/11/2022 - 1:15 PM - 1:45 PM - Tulip

Tricks of the Trade: Keeping ASTM D7169 (High Temperature Simulated Distillation) Running

Chris Goss - InnotechAlberta
Lee Marotta - PerkinElmer
Leeman Bennington - PerkinElmer

High Temperature Simulated Distillation has one of the most challenging matrices with compounds from C4 (or below) to asphaltenes.  The entire sample is injected on column, and the GC oven programs from -20 oC to 425 oC.  These create wear on the column.  Adaptations to the GC and column technology have evolved. 

This presentation will discuss the adaptation used, how they are beneficial, and tricks that can be applied to keep the system “up and running” with repeatable results.   

ASTM Method D7900 will also be examined.  D7900 gives a more accurate determination of C1 to C9 portion of the crude analysis.  When merged with D7169, gives a more accurate boiling point distribution.

Abstract # 184 - Paper
10/11/2022 - 1:05 PM - 1:25 PM - Wisteria

Using the LUMAâ„¢ as a Sensitive and Versatile Replacement for Traditional GC Detectors

Ryan Schonert - VUV Analytics, Inc.

The LUMA™ Programmable Vacuum Ultraviolet Detector has been developed to provide a balance between sensitivity, selectivity, universality, and ease of use when compared to traditional GC detectors. The LUMA™ can be easily incorporated into existing sample analysis schemes where detectors such as FID, TCD, or MS are used, and little technical training is required to start collecting data. The basics of using the LUMA™ will be discussed, including hardware information, software capabilities, and sample data gathered for various compound classes.

Abstract # 185 - Paper
10/12/2022 - 8:30 AM - 9:10 AM - Tulip

Fast and Precise Analysis of In-Service Motor Oils for Fuel Dilution and Coolant Contamination

James McCurry - Agilent Technologies

The chemical composition of in-service motor oils contains important information on the health and function of the engine.  Two ASTM methods use gas chromatographic (GC) methods to measure fuel and coolant contamination in the used oils.  ASTM D7922 combines GC with headspace sampling to simplify the separation and quantification of glycol coolants. ASTM D7593 uses GC with a unique back-flush configuration to quickly measure fuel contamination. In this presentation two systems will be described to successfully run both D7922 and D7593. Best practice techniques will be discussed to achieve fast, reliable results with a high level of precision.

Abstract # 186 - Paper
10/11/2022 - 8:15 AM - 8:45 AM - Floral Hall A1

Taking Your Routine Analysis to the Next Level

Ian Eisele - Agilent Technologies

Join us to learn about the software tools and built-in intelligence available within the Agilent ecosystem of hardware and software. OpenLab CDS paired with the 8890 GC will get you up and running smoothly and keep you running confidently. Using ASTM D3606 as an example, we will review everything from instrument configuration to autonomous system monitoring. This will include configuring multiple columns with backflush, retention-time locking, method translation, integration, and more.

Abstract # 188 - Paper
10/11/2022 - 9:15 AM - 9:45 AM - Floral Hall A1

Helium Shortage!? Alternative Carrier Gases for GC

Daron Decker - Agilent Technologies

Recently the US government announced that it will get out of the helium business allowing the private sector to develop this industry to meet the supply needs of the United States.  This has resulted in higher prices and a supply crunch of helium of which many GC users are aware and asking what can be done. This presentation will explore the options of nitrogen and hydrogen for an alternative carrier gas in GC and the implications that switching from helium brings. Various applications, detectors, column dimension changes, parameter settings and method translation will be discussed.  For those methods that ultimately prove too difficult to move away from helium carrier gas, conservation considerations will be explored.

Abstract # 189 - User Group
10/11/2022 - 12:30 PM - 1:00 PM - Floral Hall A1

Hands on experience with the Agilent 8890 GC System

Jamie Wetuski - Agilent Technologies

Learn more about Agilent GC’s on board intelligence and how it can keep your lab on track. Scheduled and self-guided maintenance offers step-by-step instructions on common maintenance procedures such as changing the septa or gold seal. New Self Aware GC features allow for on board diagnostics and troubleshooting.

Come find out how the 8890 GC can improve your lab’s workflow with this hands on experience.

Abstract # 190 - Paper
10/11/2022 - 1:00 PM - 1:30 PM - Floral Hall A1

Efforts Towards an ASTM Jet Fuel Method

Mark Kelinske - Agilent Technologies

The measurement of trace metals in petroleum feeds and its derivatives provides vital information required for running sustainable and daily petroleum operations around the world. Inductively Coupled Plasma Mass Spectrometry (ICP-MS) is used in different petroleum facilities due to its ability to perform multielement analyses, covering a broad range of concentrations as well as being robust and reliable. ICP-MS is becoming more integrated into petroleum laboratories due to its maturity and versatility.

This talk will cover our efforts towards developing an ASTM Jet Fuel method. Many interesting elements that aren’t commonly requested, including Platinum (Pt) and Pallidum (Pd), will be discussed with this new ICP-MS method. Preliminary data from our ASTM pilot study will be shared in this talk.

Abstract # 191 - Paper
10/11/2022 - 1:30 PM - 2:00 PM - Floral Hall A1

Characterization of Synthesized Iron Nanoparticles in Hydrocarbon Matrices by Single Particle (sp)ICP-MS

Mark Kelinske - Agilent Technologies

Iron-containing compounds can be problematic during the refinery of petrochemicals or the manufacture of semiconductor devices. These Iron compounds, including particles, can lead to corrosion of refinery equipment, adversely affecting the petroleum value chain. In the semiconductor industry, Fe Nanoparticles (NPs) can lead to cone defects on the surface of wafers, which cause shorting of electrical signals. Single particle inductively coupled plasma mass spectrometry (spICP-MS) is increasingly used to study NPs. Currently, most studies have focused on NPs in aqueous sample matrices, with few studies on nonaqueous matrices. One of the issues for this is the lack of hydrocarbon matrices, and solvent-compatible reference nanomaterials (RMs) to validate new methods. Two gold (Au) polystyrene-coated NP RMs in toluene and silica-shelled iron oxide (Fe3O4) alkylsilane-modified NPs in o-xylene were synthesized. spICP-MS and transmission electron microscopy (TEM) were integral to developing and characterizing the standard materials.

In this talk, we will share the spICP-MS method on the Agilent 7900 ICP-MS used to characterize the synthesized Au and Fe NP RMs. NIST crude oil standard reference material (SRM) and a NIST residual fuel oil SRM were also measured for the natural Fe NP content and spiked Fe NP content. 

Abstract # 192 - Paper
10/11/2022 - 2:00 PM - 2:30 PM - Floral Hall A1

Analysis of Wear Metals in a Variety of Lubricants in Tribological Systems referencing ASTM D5185 and using the Agilent 5900 ICP with an Advanced Valve System (AVS) and the Cetac 7400 Oil Autosampler

Paul Krampitz - Agilent Technologies

This application will focus on the methodology to run wear metals and additives in oils using a high throughput valving system and an autosampler designed to run oils.  Methodology used an Agilent 5900 ICP and a Cetac 7400 oil autosampler.  Application will include instrument setup and optimization, standard and sample preparation, quantitation, and evaluation of QC’s and NIST traceable knowns.   180 field oil samples were run for this evaluation including: new and used engine oils, transmission oils, pump drive oils, gear box oils, front and rear differential fluids, and synthetics.  Most oils were SAE 15W-40 and SAE 80W-90 fluids as well as Extreme Pressure (EP) fluids.

Abstract # 193 - Paper
10/11/2022 - 2:30 PM - 3:00 PM - Floral Hall A1

Biodiesel Applications using the Versatile Agilent 5800 ICP Including Soy Crudes, Degummed Crudes, and Finished B100 Products. BONUS – Trace Analysis in Distilled Corn Oils

Paul Krampitz - Agilent Technologies

This talk will highlight the advantages of the 5800 in running a variety of biodiesel products using organic solvents on the ICP.  Learn how to run refined and crude oils with an easy “dilute and shoot” approach.  These applications will include the analysis of sulfur as well.  Applications will reference ASTM 6751 and EN14214 for mainly Ca, K, Mg, Na, P, and S (for information).  Levels in biodiesel of these elements is well within range for the 5800 ICP.  However, techniques will be shown on how to get reliable trace analysis results of these metals as well.  Distilled Corn Oil (DCO) requires analysis in this matrix under 100 ppb for metals.  Advanced correction techniques are required to do this analysis successfully and will be shown.

Abstract # 194 - Paper
10/12/2022 - 9:00 AM - 9:45 AM - Floral Hall A1

GC Carrier Gas – How to Find and Optimizes Helium Alternatives or At Least Comfortably Live with Uncertain Helium Supply

Jim McCurry - Agilent Technologies

The hottest topic in gas chromatography today is not multidimensional GC, ultra-fast GC, or new detectors.  It is the helium supply problems and price increases impacting analytical chemists’ ability to run their current GC methods. This presentation will discuss new approaches to getting optimal GC and GC/MS performance using alternative carrier gases, but when helium is required, new technologies to continue helium use with automated conservation.

Abstract # 195 - Paper
10/12/2022 - 10:15 AM - 11:15 AM - Floral Hall A1

Method Optimization Strategies for Molecular Class Distribution of Jet, Diesel, and Light Cycle Oil Using Flow-Modulated GCxGC-FID and Hydrogen Carrier

Scott Hoy - Agilent Technologies

The evolution of fuel specifications to incorporate renewable fuels into product portfolios presents a unique opportunity for GCxGC to set a new standard for petrochemical compositional analysis. Barriers to adoption of GCxGC in production labs historically have included investment cost, lack of established methods, instrumentation footprint, and complexity of method development. The Agilent reverse-flow modulator is a low-cost and cryogen-free GCxGC solution that is simple to maintain and adds no additional instrument footprint. The recent approval of ASTM D8396 marks the introduction of standardized routine GCxGC to the petroleum QC laboratory for jet fuel analysis. This presentation will cover the conversion of D8396 from helium to hydrogen carrier, as well as strategies to expand the method to diesel and light cycle oil streams by highlighting the effects of column choice, flow parameters, and temperature programming on the separation of molecular classes.

Abstract # 197 - Paper
10/12/2022 - 8:00 AM - 8:30 AM - Tulip

Sample Precision: The path to accuracy in Refinery Gas Analyzers (RGAs).

David Strobel - Lummus Technology

On-line gas samples from R&D pilot plants often vary in flow and pressure.  These variations can cause significant changes to measured values in refinery gas analyzers (RGAs).

This presentation will discuss a commonly used technique to address on-line sample variation and share our experience with its implementation.

Abstract # 198 - Paper
10/11/2022 - 2:35 PM - 3:30 PM - Tulip

Optimize Online Sulfur Analysis In Hydrocarbons, LNG and Natural Gas With Excimer UV Fluorescence to meet ASTM Standards

Franek Olstowski - Process Insights

Excimer UV Fluorescence (EUVF) is a relatively new technology that has demonstrated an unsurpassed linear dynamic range than that achievable with conventional UV Fluorescence analyzers. This has allowed it to successfully meet the sulfur measurement and calibration requirements of regulatory standard US EPA 40 CFR Part 60.18 Subpart Ja, using a single valve and calibration standard over the entire measurement range.    EUVF has also demonstrated excellent sensitivity making it ideal for accurate, low-level measurement of sulfur in fuels, to meet required reductions in global emissions. Standards such as the American Tier III, European Euro 6, and the Indian Bharat VI set quantitative limits on permissible amounts of specific pollutants that can be released during combustion where the emission of oxides for both Sulfur and Nitrogen are regulated. Data will be presented showing successful compliance to repeatability requirements within limits set by these standards.   EUVF has also been shown to exhibit unsurpassed nitrogen interference, making it the choice for precise measurement of low sulfur levels required by these regulations, particularly when high nitrogen content is present. EUVF is now a proven technology with ATOM Instrument, part of Process Insights, being the only manufactured brand incorporating this superior version of UV fluorescence in their analyzers.

Abstract # 199 - Paper
10/11/2022 - 1:35 PM - 2:00 PM - Bluebonnet

Key advantages of Time Domain NMR (TD-NMR) analysis of polypropylene samples

Gabriel Villarreal - Lummus Technology

The implementation of TD-NMR (Time-Domain NMR) allows for the fast and precise measurement of key properties of polymers in comparison to more manual centered techniques.  Properties that indicate final product quality, catalyst functioning and process efficiency can be understood through this powerful technique. 

This proposal endeavors to share an example of an analysis performed on polypropylene samples utilizing TD-NMR in order to determine xylene solubles.  The principles of this technique coupled with the properties of the sample are presented.  The basics of instrument setup and calibration will be presented as well.

Abstract # 200 - Paper
10/11/2022 - 2:50 PM - 3:20 PM - Bluebonnet

Advanced Process Control and Optimization of Canadian Heavy Crude Oil Distillation Using Online Process NMR Rapid Crude Property Measurements.

Shashi Mistry - Suncor Energy
Paul Giammatteo - 4IR Solutions, Ltd.

Since its installation in 2018 at the Sherwood Park, Alberta refinery, on-line Process Nuclear Magnetic Resonance (NMR) continues to provide real-time crude assay and property measurements on Canadian bitumen heavy crude feeds including cut points, distillation fractions, densities, asphaltenes, water content, etc.  This presentation will provide an overview of the installation, measurements, and integration into the refinery’s control and optimization programs. Reliability of the NMR system contributing to improved refinery operational and economic performance will also be presented.

Abstract # 201 - User Group
10/11/2022 - 8:20 AM - 9:20 AM - Iris

Benefits from ultra low range chlorine monitoring and control

Jody Faust - HACH

A user group focussed on the benefits of monitoring and controlling free residual chlorine at ultra low levels.  Mainly the discussion will be focussed on applications in RO feedwater and permitted wastewater discharge.  Previous to the introduction of new equipment from Hach, the monitoring of free chlorine at levels less than 3-4 ppm was dubious and unreliable.  Now we have the ability to monitor for free chlorine online and continuously with a low limit of 8 ppb.  We will discuss the application of this new technology and how it may benefit you operations.

Abstract # 202 - User Group
10/12/2022 - 8:00 AM - 8:30 AM - Iris

Surface Area with Velocity: Fast and Accurate Gas Sorption Measurements

Nathalia Prieto - Anton Paar
William Davis - Anton Paar

The Anton Paar Nova series of instruments is capable of quickly and accurately measuring the BET surface area of powders and porous materials. An analysis time of 20 minutes for four simultaneous BET measurements with a reproducibility of < 2% can be obtained. This will be demonstrated live on a Nova instrument and the time saving and unique features of the instrument will be discussed.

Abstract # 203 - Paper
10/12/2022 - 3:30 PM - 4:00 PM - Iris

See the tree and the forest: high performance helium-free XRF for Ultra Low Sulfur and Chlorine

Taco van der Maten - MalvernPanalytical

As ASTM and ISO regulations around sulfur content become more stringent, performance-based norms are more important than ever. One example is ISO 13032, soon to be updated. Meeting these and equivalent performance requirements with EDXRF previously required expensive helium.

But no longer. The highly sensitive Epsilon 1 ULS from MalvernPanalytical meets the requirements without any helium – and has an impressive LLD below 1 ppm. Moreover chlorine can be measured at low ppm levels next to percentage measurements of sulfur, for example in spot crude. Examples and details will be presented.

Abstract # 204 - Paper
10/12/2022 - 9:25 AM - 9:55 AM - Iris

A Reintroduction to the PAC OptiFuel

April Zamora - PAC

The analysis of diesel and gasoline has become a cumbersome task for most laboratories across the globe due to the number of instruments that are required to get a full panel of data. With the PAC OptiFuel, an FTIR spectroscopy analyzer, analysis of these fuels can be performed in under 3 minutes with one instrument. FTIR technology is an established analytical tool that has some distinct advantages when used for the analysis of petroleum mixtures. The OptiFuel is designed to meet the needs of all types of laboratories ranging from terminals to research with one touch of a button analysis.

Abstract # 205 - Paper
10/11/2022 - 8:00 AM - 8:40 AM - Tulip

Oil Field Waters using a new plasma interface (DSOI) for ICP-OES analysis with a focus on Phosphorous & Clorine

Dion Tsourides - SPECTRO Analytical Instruments

The ability to measure Phosphorus and Chlorine is critical in Oil Field Waters. Traditionally it required multiple analytical techniques and/or multiple samples preparations. This presentation will discuss the advances in plasma viewing using a Dual Side On Interface which eliminates the need for multiple analysis of the same sample while simplifying the process. Cost and maintenance savings using this spectrometer system is typically >$5000 per year.

Abstract # 206 - Paper
10/11/2022 - 12:20 PM - 12:40 PM - Iris

UV-Fluorescence and Chemiluminescence to Control Sulfur and Nitrogen in the Petrochemical Revolution

Karl Kuklenz - PAC
Koen Vink - PAC

The petrochemical revolution is already well underway, with petroleum naphtha playing a vital role as the gateway to several of the key chemical building blocks.  Of the five major petroleum manufactured products, only naphtha is predicted by analysts to significantly grow its global demand by 2050.  This demand coupled with the tight tolerances required for petrochemical feedstocks will shift the focus of production into new areas of control, both in the laboratory and in process.  UV-fluorescence and chemiluminescence are methods that are well suited to the need to control sulfur and nitrogen, and can be scaled from the laboratory to the process with confidence.

Abstract # 207 - Paper
10/11/2022 - 1:30 PM - 2:00 PM - Daffodil

GC Carrier Gases: Finding the best option for your lab

Nicole Lock - Shimadzu Scientific Instruments, In

Acquiring helium to be used for carrier gas on GC and GCMS systems continues to be a challenge.  Issues with supply are requiring laboratories to rethink not only their analytical methods, but also their instrument processes.  Alternative carrier gases can be used for many methods, but there are times when the only option is helium.  As an instrument operator, we need to understand the possibilities available to us. Knowing the different options for carrier gases, the pros and cons of each gas, and what to do when helium is the only option is key. 

Abstract # 208 - Paper
10/11/2022 - 9:00 AM - 9:30 AM - Daffodil

The Advantages of Client Server Data Management (CDS) in Small to Medium Labs”

Jeffey Werner - Shimadzu Scientific Instruments, Inc

Today data integrity and security are of the utmost importance in laboratories large and small.  In order to meet the needs of the various industries, many customers are exploring Chromatography Data Software (CDS) that incorporates levels of security and integrity not previously used.  This presentation will explore the Lab Solutions Client Server software and the advantages to small and medium laboratories as they grow and change.  In addition to the data integrity and security that a client server software offers, there is also a convenience piece not generally available in workstation versions of a CDS.  We will explore these options as well as the expandability of the system.

Abstract # 210 - Paper
10/11/2022 - 11:30 AM - 12:00 PM - Daffodil

X-ray Fluorescence Analysis of Petrochemical Matrices

Joel Langford - Shimadzu Scientific Instruments, Inc

Quantifying elemental content in petrochemical matrices is important for a variety of reasons including, health, compliance, and its influence on chemical and physical properties. There are multiple established methods for elemental analysis, however, for reasons such as speed, and simplicity, X-ray fluorescence spectroscopy is considered as one of the “go-to” methods. A new Energy Dispersive X-ray fluorescence system, called the EDXRF-7200, that has higher sensitivity and speed compared to previous generations of EDXRF, has been released in the United States. In this talk, we will concentrate on how the EDXRF-7200 improves over previous EDXRF technology, and the implications of this improvement with regards to petrochemical analysis.

Abstract # 212 - Paper
10/11/2022 - 11:00 AM - 11:30 AM - Daffodil

TOC Analysis: Do You Know What You Are Reporting

Ricky Frnka - Shimadzu Scientific Instruments, Inc

Performing organic carbon analysis on wastewater and process streams is vitally important to the petrochemical industry.  Properly maintaining and troubleshooting instrumentation is imperative to providing reliable analytical results.  Several factors play a key role in the proper operation of a TOC system.  These factors, causes, resolutions and available options will be discussed.

Abstract # 213 - Paper
10/11/2022 - 2:00 PM - 2:30 PM - Daffodil

Metrology A Good Program for Your Lab

Ricky Frnka - Shimadzu Scientific Instruments, Inc

Metrology System Helping to Ensure the Integrity of Your Data   Performing analytical testing and providing data are the two important responsibilities of a laboratory.  Ensuring data integrity is a top priority as data is the finished product of labs.  Properly calibrating and maintaining instrumentation along with documentation of these events are imperative to providing reliable analytical results.  Tips on setting up a system to provide a framework will be discussed.

Abstract # 214 - Paper
10/11/2022 - 2:30 PM - 3:00 PM - Daffodil

Improved anions analysis – impact of newer technologies in older contaminants.

Quoc-Huy Ho - Shimadzu Scientific Instruments, Inc

Fast and robust analysis of anions in environmental samples is essential for environmental laboratories due to the short turn-around-times required for the analysis of nitrate and nitrite in methods EPA 300 and 300.1. When analyzing samples with diverse and variable composition for nitrate and nitrite together with some of the other targets from these methods (e.g., F-, Cl-, Br-, PO4-, and SO4- from EPA 300), laboratories may run into challenges. For example, high concentrations of chloride in the matrix can mask the presence of nitrite, preventing the detection of the later by suppressed conductivity detector required in the method. Hence, two or more injections may be needed for obtaining the required results, resulting in decreased productivity. In this work, we first optimized the method conditions to maximize lab productivity and turn-around-time for  the analysis of the seven anions targeted in EPA 300 in a run-to-run time of 4.5 minutes (4.0-minute gradient). In an attempt to further increase the efficacy of the method, we evaluated two approaches to eliminate the need for sample-reruns when results from various anions are outside the calibration range or interferences are present: 1) lowering the injection volume (down to 0.2 µL) to avoid the need for sample dilutions (in- or off-line) and 2) using a conductivity and UV detectors in-line to detect nitrite in the presence of high concentration of chloride. In this presentation we will present the results from the method performance evaluation including but not limited to linearity, sensitivity, and reproducibility.

Abstract # 215 - Paper
10/11/2022 - 3:00 PM - 3:30 PM - Daffodil

The degradation and associated contaminants of microplastics in marine environments

Zhanfei Liu - University of Texas at Austin

Microplastics, defined as those in size <5mm, are becoming more abundant in marine waters due to the continuous discharge and their resistance to environmental degradation, and they are harmful to the organisms and ecosystems in environments. It is, therefore, critical to understand how plastics degrade biologically and photochemically, and how contaminants, such as polycyclic aromatic hydrocarbons (PAHs) and polychlorinated biphenyls (PCBs), are sorbed to microplastics. In this talk, I will briefly summarize several of my recent or on-going projects related to microplastics, including nurdles pellets along Texas coasts and their associated PAHs and PCBs. Also included are results of plastic degradation from laboratory photooxidation and biological degradation in the deep sea. I will also talk about how state of the art analytical tools, including microscope FTIR, pyrolysis GC/MS and gel permeation chorography, are used to analyze plastic samples.

Abstract # 216 - Paper
10/11/2022 - 1:00 PM - 1:30 PM - Daffodil

Shimadzu’s Analytical Solutions for the Hydrocarbon Processing Industry and Customer Case Studies

Raj Makhamale - Shimadzu Middle East & Africa FZE

Shimadzu offers a complete suite of instruments applicable to the hydrocarbon processing industry (HPI), including gas chromatography and applicated systems, GC/MS, elemental spectroscopy, TOC, and more. This presentation will provide an overview of Shimadzu’s complete analytical solutions for the HPI as well as case studies in customer success with major global installations at refineries and chemical facilities.  Particular attention will be paid to instrumentation applicated to industry standard test methods and support of large installation bases at these types of facilities.

Abstract # 217 - Paper
10/11/2022 - 9:10 AM - 9:30 AM - Tulip

Carrier Gas: Moving to Hydrogen or staying with Helium? A Solution to Support both choices

Amit Gujar - Thermo Fisher Scientific
Daniela Cavagnino - Thermo Fisher Scientific

Disruption in the Helium supply chain continue to pressure analytical laboratories to find alternative solutions for their carrier gas requirements.  Hydrogen can be an alternative but requires method modifications, re-validation, safety protocols and may not work with specific samples.  When Helium is the best option, reducing consumption becomes mandatory. Thermo Fisher Scientific developed a new option for its Split/Splitless inlets, the HeSaver-H2Safer kit. HeSaver mode extends the lifetime of a He cylinder 350% by optimizing Helium consumption. The H2Safer mode ensures safe operation and optimizes the Hydrogen consumption - a benefit when using capacity limited Hydrogen generators.

Abstract # 218 - Paper
10/11/2022 - 9:30 AM - 10:00 AM - Daffodil

Fuel Cell Analysis by Gas Chromatography

Allison Mason - Shimadzu Scientific Instruments, In

The emphasis on “Green” chemistries has rejuvenated interest in alternative fuels. Many alternative fuels are generated by catalytic fuel cells or biological reactions which can produce unwanted by-products. As with any fuel source, quantifying impurities is of the utmost importance to increase the efficacy of the fuel and prevent damage to systems using the fuel.  An applicated gas chromatographic system was developed to measure common light organic and inorganic impurities in alternative fuels.

Abstract # 219 - Paper
10/11/2022 - 8:00 AM - 8:20 AM - Rose

Ion Chromatographic method for triethylamine (TEA) extracted from plastic films

Isaac Negrete - Dow
Stephen Fosdick - Dow

Along with ever-improving sensitivity and performance of available analytical methodologies comes the challenge of lower and lower detection and quantitation limits. While hyphenated techniques present clear solutions to a variety of analytical challenges, this presentation is an example of how fundamental understanding of technology, appropriate flow paths, and column selection can achieve improved results. This is demonstrated by a method for identifying and quantitating extracted triethylamine from plastic film washes using a Dionex IonPac CS20 IC Column, achieving ng/L with suppressed conductivity detection.

Abstract # 220 - Paper
10/11/2022 - 2:00 PM - 2:20 PM - Bluebonnet

Use of the JFTOT IV Jet Fuel Thermal Oxidation tester with renewable fuels

Ian Mitchell - Petroleum Analyzer Company

ASTM D3241-20c is the standard test method for Thermal Oxidation Stability of aviation turbine (jet)  fuels. This is an important test that ensures the sampled fuel does not leave excessive deposits onto a heated surface such a jet engine components. As such this a key test ensuring the suitability of jet fuels and has been in use for many years. The aviation industry is moving to increase the use of Sustainable Aviation Fuel (SAF). As part of this process, the SAF fuels also need to be tested for Thermal Oxidation Stability. PACs JFTOT IV Thermal Oxidation Stability testing instrument has been adapted and tested to ensure the new renewable fuels can be run using the same instrument and method. Data will be presented showing the modifications that were implemented and the testing that was conducted to ensure continued compliance with the ASTM method requirements.

Abstract # 221 - Paper
10/12/2022 - 9:30 AM - 10:00 AM - Bluebonnet

Real-time Flare Gas Analyzers for 40 CFR 60 and 63- EMACT, MONMACT and MACT CC- What Analyzer is Best for Your Flare Plan?

Chuck DeCarlo - Process Insights
Monique Murphy - Process Insights
Chris Williams - Process Insights

Flare compliance can be challenging. An optimal flare plan depends on strategically matching technology and procedures to each of the regulatory requirements that apply. Based on the location of the plant and the EPA regulatory category, the analyzer portion of the flare plan will require one or more of several measurements, including Net Heating Value (aka. BTU value), H2S, Total Sulfur, hydrogen, and even speciated hydrocarbons for HRVOC. This talk will review three of the leading solutions for flare gas analysis: mass spectrometers, calorimeters, and total sulfur analyzers. We’ll look at data and the configuration details important to successful flare gas analysis, and address how other sites are using these analyzers to prepare for the EMACT and MONMACT deadlines coming up in 2023.

Abstract # 222 - Seminar
10/11/2022 - 11:15 AM - 11:45 AM - Floral Hall A2

Screening for PFAS and Other Fluorinated Compounds using Combustion Ion Chromatography

Kirk Chassaniol - Thermo Fisher Scientific

With the number of environmentally relevant per and polyfluorinated alkyl substances (PFAS) compounds and precursors that cannot yet be analyzed continuing to increase, there is a need to develop suitable analytical methods for their detection. Many PFAS are not accounted for by existing analytical methods.  A single analytical workflow that would allow for a direct determination of as many PFAS as possible. Automated combustion ion chromatography (CIC) can be used to determine organic halogen contaminants, such as AOX (X = F, Cl, and Br). 

Abstract # 223 - Paper
10/11/2022 - 12:45 PM - 1:15 PM - Tulip

Easy analysis of hydrocarbon group types in Jet Fuel with GCxGC

Jorge Colonia - PAC L.P.

Quality of Jet Fuel is key to flight safety. It’s composition, in particular aromatics content, is regulated to ensure proper combustion characteristics and compatibility with aircraft fuel systems. As the aviation industry moves to lower carbon intensity, new fuel types emerge which differ in composition from traditional petroleum-based fuels. Legacy test methods struggle to meet performance characteristics required to test these sustainable aviation fuels (SAF). A new test method (ASTM D8396) was developed, based on comprehensive two-dimensional GC. This method provides detailed hydrocarbon group-type composition, whilst the simplicity of the flow-modulated setup allows implementation in routine lab environments.

Abstract # 224 - Paper
10/11/2022 - 8:45 AM - 9:10 AM - Rose

Resolving a Complex Problem in Petrochemical Facilities Using PY-GC/MS and PY-FTIR

Brent Moore - Moore Analytical

An unknown white powder was continuouesly plugging the filters in an Aqeous Process Line causing the Unit to shut down for maintenance. Samples were rushed to the lab for analysis.  Initial testing by the plant lab did not determine what the white powder was.  Introduction of this powder sample using Pyrolysis to both a GC/MS and FT-IR, and using the libraries of both instruments, helped determine what the precipitate was and where it was coming from.

Abstract # 225 - Paper
10/11/2022 - 8:30 AM - 8:50 AM - Bluebonnet

Creating Controlled Humidity for Calibrating Gas Monitors, Sensors, and Detectors

Danet Vrazel - KIN-TEK Analytical Inc

Many industries monitor atmospheric conditions to measure gas pollutants in humid environments.  Varying levels of ambient humidity can interfere with gas monitors and sensors and diminish response factors. Calibration of gas monitoring and detection devices should relate to ambient conditions and include the percent relative humidity (%RH) consistent with surrounding areas. Creating various %RH levels in a zero-gas stream or a calibration gas stream can be challenging and ineffective if done improperly.  A permeation system that supplies accurate calibration gas with controlled %RH at varying levels is an effective solution for calibrating or exposing monitors, detectors, and sensors at ambient conditions.

Abstract # 227 - Seminar
10/11/2022 - 9:10 AM - 9:55 AM - Bluebonnet

Laboratory Optimization and Improvement

Jeanne Mensingh - Labtopia

Reducing costs and streamlining laboratory processes are necessary activities for any organization. This presentation will provide an overview of areas to review during a business optimization project with examples. These real-world examples will provide enough information for the laboratory manager or chemist to take back to the laboratory and make improvements that directly influence cost savings, employee retention, productivity, and efficiency.

Abstract # 229 - Paper
10/11/2022 - 12:20 PM - 12:45 PM - Tulip

Comparing Pyrolysis-GC-MS to Pyrolysis-FT-IR on Polymer Sample Analysis

Brent Moore - Moore Analytical

The use of Pyrolysis GC/MS and FT-IR to solve complex analytical problems in a polymer manufacturing facility.  The combination of these techniques provide a fast resolution to identify contamination occuring in the process stream.

Abstract # 230 - Paper
10/11/2022 - 12:00 PM - 12:20 PM - Iris

Determination of Additive Elements in Lubricating Oils according to ASTM D4951 with HR ICP-OES

Jessica Gantt - Analytik Jena US LLC

Lubricating oils are the lifeblood of oil-wetted machinery. In this study, ASTM D4951 method is demonstrated with Analytik Jena’s PlasmaQuant 9100 Elite, equipped with an organic sample introduction kit. Linear calibrations were obtained with correlation coefficients greater than 0.9999 for all elements. ASTM D4951 expects detectability in the low mg/kg range for most elements to be sufficient. The method detection limits (MDL) of all analytes are below 90 µg/kg. To evaluate the long-term stability, 50 quality control samples were analyzed continuously. For all the elements, the recovery of quality control standards was within ± 5 % of the expected value.

Abstract # 232 - Paper
10/12/2022 - 11:05 AM - 11:25 AM - Tulip

Analysis of Elemental Impurities in Diesel and Gasoline by HR ICP-OES

Jessica Gantt - Analytik Jena US LLC

Diesel and gasoline are among the most challenging samples to be analyzed by ICP techniques. Due to the vertical plasma geometry of the V Shuttle Torch and the unique plasma performance of its high-frequency generator, direct analysis of undiluted diesel and gasoline proved feasible for the analytical routine on the Analytik Jena PlasmaQuant 9100 Elite. The limits of detection in the range of 1 ppb are easily achieved for most analytes, which ensures the precise and accurate determination of the required limits. Carbon-based spectral interferences are successfully removed by the high spectral resolution of the High-Resolution Optics. Excellent method robustness was confirmed by a continuous aspiration test.

Abstract # 233 - User Group
10/11/2022 - 12:30 PM - 1:15 PM - Bluebonnet

Round Table Discussion: Trouble finding talent after the “Great Resignation”?

Greg Berry - Labtopia Staffing
Katie Tyer - Labtopia Staffing

Hiring employees in 2022 has shaped up to be a continuation of 2021’s “Great Resignation” and challenges still persist on finding the right candidate for your organization. Labtopia Staffing hears concerns from clients about staff shortages, trouble finding qualified candidates and employee retention. We will discuss what we are hearing from candidates, why they are leaving their current employers and what they are seeking in a new position.  We will open this up to discussion with participants on what has worked (or not worked) to attract new talent to your organization and ways to retain those that are important to your business.

Abstract # 234 - Paper
10/11/2022 - 9:25 AM - 9:45 AM - Wisteria

Comparison of Gas Chromatography Vacuum Ultraviolet detectors

Dion Boddie - Lummus Technology
Jean-Francois Bourny - Lummus Technology

Gas chromatography Vacuum UltraViolet spectroscopy (GC-VUV) is fairly new to our industry. The first bench top detector was available in 2014. Since then, many ASTM methods have been developed and continue to be added. This presentation will be comparing the three GC-VUV detectors that we use at Lummus Technology. We will include the current ASTM methodology and also some enhanced detections for pyrolysis oil and other samples that can be challenging.

Abstract # 235 - Paper
10/12/2022 - 9:25 AM - 9:45 AM - Wisteria

New Solvents for Routine Polyethylene NMR Analyses – Moving Past Deuterium

Joseph Romaniuk - Dow Chemical Company

Polyethylene is one of the most important industrial polymers, and NMR is essential to evaluating its molecular structure by measuring co-monomer content, sequence distribution, unsaturation, and long chain branching.1 Routine polyethylene NMR analyses require the use of specialized, deuterium-based solvents. While necessary for locking and shimming the NMR field, these solvents are expensive, subject to supply interruptions, and often hazardous. Here, we share our progress at Dow Chemical to find safer, deuterium-free solvent systems for routine polyethylene NMR.

1. W. deGroot, D. Gillespie, R. Cong, Z. Zhou, R. Paradkar, Handbook of Industrial Polyethylene and Technology, Scrivener Publishing LLC, 2017, 139.

Abstract # 236 - Paper
10/11/2022 - 1:25 PM - 1:45 PM - Wisteria

Sensitive and Selective Detection of BTEX Compounds Using the LUMAâ„¢ Programmable Vacuum Ultraviolet Detector

Ryan Schonert - VUV Analytics, Inc.

While fuels and feedstocks are often characterized by their overall composition, certain individual compounds within samples, such as benzene, toluene, ethylbenzene, and xylenes, may be targeted for a more detailed analysis. Such compounds have specific tests dedicated to their detection and quantitation, and they are usually measured at trace levels.  The LUMA™ Programmable Vacuum Ultraviolet Detector offers a simple, sensitive, and cost-effective solution for identifying and quantifying targeted compounds, and it can be easily incorporated into existing analysis schemes where traditional GC detectors are used.    

Abstract # 237 - Paper
10/11/2022 - 1:45 PM - 2:10 PM - Tulip

Polyarc System Use Case for Quantification of Reaction Kinetics for Sustainable Aviation Fuel

Connor Beach - Activated Research Company

There is a race against the clock for faster analytical capabilities to advance reaction chemistry for sustainable fuels, plastics, and bioproducts. We will discuss how the Polyarc System enables researchers to quantify functionalized organic compounds without calibration. The Polyarc System utilizes a post-GC column two-step microreactor to convert all organic analytes to methane for detection with an FID. This allows for a faster and better understanding of reaction kinetics through a direct measurement of the carbon mass balance. Important steps have already been taken to better understand the chemical reaction pathway to create sustainable aviation fuels from volatile fatty acids as a feedstock.

Abstract # 238 - Workshop
10/11/2022 - 1:15 PM - 2:00 PM - Rose

Jumpstart Your Lab Training Program!

Gretchen McAuliffe - Labtopia

Development and maintenance of laboratory training programs can be a challenging task. Though laboratory management generally understands the necessity for such programs, training is often not consistent nor sufficiently comprehensive, with the result that it is frequently cited as a deficiency in laboratory audits.

A well-defined and documented laboratory technician training program is essential, with the overarching goals being to cultivate competent and well-trained employees, and to establish a role-based training matrix so that supervisors can ensure employees develop the skills necessary to perform their assigned tasks.

We will discuss how to develop this essential blueprint for a laboratory training program, then move to how to maintain the program once established. We will also address the value of engaging with a consulting partner that can provide the momentum necessary to ensure project completion, as well as additional tools that will jumpstart your lab's training program.

Abstract # 239 - Paper
10/11/2022 - 1:15 PM - 1:35 PM - Bluebonnet

Simple methods for group-type quantitation of hydrocarbons using flow-modulated GCxGC-MS/FID

Christina Kelly - LECO Corporation
Joseph Binkley - LECO Corporation
David Borton - LECO Corporation
Mark Merrick - LECO Corporation

Reference aviation and diesel fuels were tested along with gravimetric standards on a reverse fill-flush GCxGC-FID system following ASTM D8396, demonstrating robust hardware and simplified method parameters that reliably provide full transfer of analytes from the primary to secondary GC column. Additional sample characterization utilized a prototype GCxGC-TOFMS/FID instrument equipped with a novel splitter design ensuring a consistent split ratio between the MS and FID detectors to avoid erroneous area percent determinations and a novel peak alignment algorithm simplifying identification of FID peaks using corresponding MS spectra to assist in drawing regions for more accurate group-type quantitation of chemical classes.

Abstract # 242 - Paper
10/11/2022 - 8:50 AM - 9:10 AM - Bluebonnet

Creating Moisture Gas Standards

Spencer Hallaway - KIN-TEK Analytical, Inc.

Removing moisture concentration levels down to ppm, ppb, and ppt levels is critical in many manufacturing, electrical, and medical processes. Moisture sensors can be used to determine if an environment is optimal for the process but calibrating the sensors with accurate moisture standards can be daunting. Water moves from areas of higher concentration (such as the atmosphere) to areas of lower concentration (such as the moisture standard) by permeation and diffusion. It is also a polar compound that sticks to almost any surface that has a charge. Creating a Moisture Standard can be done if approached correctly.

Abstract # 243 - Seminar
10/11/2022 - 2:15 PM - 3:05 PM - Iris

QC/EZ Product Showcase: SQC According to D6299 Demonstrated With The Newest SAAS Solution

Josh Burkhalter - Baytek International

Baytek International brings you the same powerful QC workflow from QC/PLUS, now in a lighter package.  QC/EZ is the world’s first subscription-based software solution capable of performing ASTM D6299, EPA Part 1090 Compliance, along with a full suite of additional control charting options.   QC/EZ is tailored for labs both large and small, across all industries. As EZ as selecting your subscription level, logging into the QC/EZ web-application and enjoying the fully functioning SQC system the same day.  We will demonstrate how simply a user can join QC/EZ, load data and fully utilize the solution; all while demonstrate the ASTM D6299 workflow and the many features of QC/EZ. 

Abstract # 244 - Workshop
10/12/2022 - 8:30 AM - 9:25 AM - Iris

Resolving Your Control Charts Ailments: An Interactive SQC Workshop

Josh Burkhalter - Baytek International

Have you ever wanted to pick someone’s brain about control charting issues you’ve experienced?  Do you have a problematic control chart, or just have some questions that have gone unanswered?  

Baytek SQC Consultants will lead an interactive discussion with workshop attendees on topics relating to challenges with SQC systems.  Attendees will be invited to share their own experiences managing their SQC programs.  Attendees may bring example charts to the workshop; and are encouraged to email examples and questions to the moderators if they wish to remain anonymous. 

Abstract # 246 - Seminar
10/12/2022 - 9:30 AM - 10:30 AM - Daffodil

Keep it Simple: Useful Tips for Accurate & Reliable Karl Fischer Analysis

Kerri-Ann Blake - METROHM USA

Is your Karl Fischer titration taking too long?  Does poor reproducibility slow down KF method validation?  Have you optimized sample preparation to ensure total moisture is titrated?  KF titration is a common laboratory measurement used for many different oil and refinery products.  Optimizing KF measurements is key to increasing lab productivity and maintaining product quality and process control. While a moisture measurement is straightforward, getting the right result quickly and reliably can be a challenge.  Attend this talk to learn the importance of parameter optimization, reagent selection and sample preparation to get reliable and accurate moisture analysis.

Abstract # 247 - Seminar
10/12/2022 - 9:00 AM - 9:30 AM - Daffodil

Low Moisture Analysis in Chemical Production

Elena Hagemann - METROHM USA

The analysis of moisture in chemical production and solvent recovery is commonly performed by coulometric Karl Fischer titration (KFT) in an offline wet chemistry lab. The time required for measurements and manual sampling often cause a lag between receiving data and process implementation. This results in either unnecessary drying steps or insufficient drying, increasing costs. A better solution is online NIR measurement. However, NIR instruments often require significant effort to calibrate, especially at the levels required for many high-purity streams.
In this talk, we demonstrate a system that eliminates the calibration effort by automatically building and checking the calibration, without manual sampling. This capability allows moisture measurement systems to be calibrated at the factory down to approximately 5 ppm and installed in pipelines and reactors without additional calibration effort.

Abstract # 248 - Seminar
10/12/2022 - 10:30 AM - 11:00 AM - Daffodil

Optimized Amines Separation to Increase Corrosion Monitoring Accuracy

Jay Gandhi - METROHM USA

Monitoring corrosion is key to maintaining successful long-term operation of oil pipelines and refineries. Amines are routinely added to neutralize hydrogen sulfide vapor for transport of crude to the refinery and are typically used to strip hydrogen sulfide, carbon dioxide, and other acidic gases in the refining process. However, too much amine present in the wrong location can increase corrosion rates. Therefore, it is in the industry’s best interest to monitor these corrosion sources and work is underway at ASTM to develop a standard practice for extraction of water-soluble amines in crude oil. This talk addresses the impact of amines on crude refinement and the versatility of ion chromatography to monitor these species.

Abstract # 249 - Seminar
10/12/2022 - 3:00 PM - 3:30 PM - Daffodil

Applications and Techniques Using Combustion Ion Chromatography

Jay Gandhi - METROHM USA

Not all samples are amenable to direct injection into an ion chromatograph.  In such cases, combustion ion chromatography can be an important tool for the analysis of halogens and sulfur in a variety of sample matrices. Basic concepts in combustion ion chromatography (Combustion IC, CIC) analysis will be introduced with practical industry-based applications. Topics will include an overview of ASTM methodologies in the petrochemical industry that feature Combustion IC, as well as a look at analyzing polymer processing additives.  Exemplary data from these methods will be presented. 

Abstract # 250 - Seminar
10/12/2022 - 2:15 PM - 3:00 PM - Daffodil

The Changing PFAS Landscape and Upcoming EPA Method 1621

Jay Gandhi - METROHM USA

What we know about PFAS compounds is changing every day, as the list of compounds continues to grow and be detected in more products and the environment.  Historically, targeted LC-MS/MS methods have been used to detect and quantify a limited list of these compounds, though there is increasing interest in non-targeted methods, which look at total fluorine and give a better picture of the overall impact.  The US EPA has acknowledged this shift in thinking with the proposal of method 1621, which screens for adsorbable organic fluorine (AOF) using combustion ion chromatography (CIC).  In this talk, details of upcoming method 1621 will be discussed along with an optimized sample prep and CIC solution.    

Abstract # 251 - Paper
10/12/2022 - 2:00 PM - 3:00 PM - Floral Hall A1

Proposed Revision and Expansion of ASTM D7845

George Gonzalez - Agilent Technologies

This presentation provides the current status of ASTM work item #56072 method development to revise ASTM D7845. The proposed expansion includes FAME, fatty acids, fatty acid monoglycerides, Bisphenol A, Bisphenol F, and benzenediols. The presentation will consist of test method apparatus, chromatograms, test method performance, and the path forward for development at ASTM. 

Abstract # 252 - Paper
10/11/2022 - 8:45 AM - 9:15 AM - Floral Hall A1

How GPC fits into the HPI Workflows

Sue D'Antonio - Agilent Technologies
Nik Lau - Field Applications Chemist

  In this talk we will show GPC as a tool for the HPI analyst. This will be an interactive session with practical tips and tricks for the end user. Modes of detection such as ELSD, VWD and RID will be discussed.  

Abstract # 253 - Paper
10/12/2022 - 10:25 AM - 10:45 AM - Iris

Analysis of Fatty Acid Methyl Ester (FAME) in Fuels via FTIR

Samantha Nania - PerkinElmer

Biodiesel is a fuel made from renewable bio sources such as vegetable oils.  Advantages of biodiesel usage include reduction of emissions, namely carbon monoxide and particulates. While these benefits are attractive, biodiesel can only be used in specialized engines. Therefore, analyzing FAME concentrations in diesel is critical for quality control and verification of blended biodiesel and fuel labeling. There are various EN and ASTM methods for analyzing FAME concetration in diesel. This talk will discuss the various methods used for analzying FAME via infrared spectroscopy and the benefits of each method.

Abstract # 254 - Paper
10/12/2022 - 9:10 AM - 9:40 AM - Tulip

Easy Techniques to Identify What is in Your Products

LEE MAROTTA - PerkinElmer
Leeman Bennington - leeman.bennington@perkinelmer.com

Gas Chromatography (GC) sample introduction techniques such as headspace (HS) and automated thermal desorption (ATD) are very easy useful tools for the investigation of compounds in many matrices and products whether the requirement is product quality or toxic compound investigation.  

There are several benefits using HS and ATD to attain information.  They are less labor intensive providing enhanced productivity; they optimize sensitivity because they automate concentration; and they require little to no solvents rendering them environmentally friendly.   

Information that can be attained using these technologies and the sample types will be discussed.  In addition, which one is best to use.

Abstract # 255 - Seminar
10/12/2022 - 10:05 AM - 10:25 AM - Tulip

Dual Application Process GC Supporting 2 Sample Streams

Roger Bustos - Dow Chemical

Application of on-line analytical measurements to observe chemistry in near real-time allows the end-user of the data to more easily link "cause and effect." The agility and power of liberating the technology affords end-users a means to determine the conditions for optimum yield, ensure process control, understand process upsets, and characterize unknown chemistry with urgency and sample integrity not possible by conventional “grab sample” analysis.  This application-laden presentation will describe the use of a single Siemens Maxum Edition II process GC with dual applications. Each application was independently controlled by Siemens’ GC Portal (GCP) and evaluated for linearity, accuracy, and precision for 12 unique components to gather analytical information needed to better understand, optimize, and probe chemical problems.

Abstract # 256 - Paper
10/12/2022 - 9:45 AM - 10:05 AM - Wisteria

Waters RADIAN ASAP: User Evaluation and Industrial Applications

Junho Jeon - Dow Inc.
Janece Potter - Dow Inc.
Anthony Gies - Dow Inc.
James Alexander - Dow Inc.
Ron Tecklenburg - Dow Inc.
Bryan Katzenmeyer - Waters
Zach Hardie - Waters
Spencer Harvis - Waters
Greg Patten - Waters
Damian Morrison - Waters
MIchael Jones - Waters
Cristian Cojocariu - Waters

Atmospheric Solid Analysis Probe (ASAP) has been popular last decades for insoluble or high boiling material analysis with the development of atmospheric pressure chemical ionization (APCI).  Dow’s Core R&D Analytical Science (AS) and Waters Technologies Corporation (Waters) collaborated the test of the new-to-market instrument specifically for industrial applications (Waters RADIAN) in 2021-2022. In this evaluation, Dow AS performed multiple sample analyses using RADIAN including glycols, polyols, additives, and polyurethane prepolymers. The data were compared with multiple other products for characterization purposes. Compared with conventional thermal desorption/pyrolysis (TD/Py)-gas chromatography/mass spectrometry (GC/MS), the results indicated promising potential applications for time-efficient and screening procedures of solid and non-soluble sample analysis. In this presentation, Dow AS also shares gained knowledges about the operation of RADIAN for high boiling liquid/solid/oligomeric/polymeric sample analyses without additional processing/preparation as merits and the gaps from the newly developed instrument under industrial settings.       

Abstract # 257 - Paper
10/11/2022 - 2:20 PM - 2:50 PM - Bluebonnet

Navigating the Transition from Helium as a Carrier Gas

Leeman Bennington - PerkinElmer

Chromatographers use approximately 7.9% of the available helium resources per year.  Helium costs are rising sharply; and shortages, are hindering productivity and profits.    This presentation will focus on attaining high analytical performance using alternative carrier gases such as hydrogen and nitrogen in petroleum and environmental applications, as follows:  

·         New state-of-the-art technology to enable the safe usage of hydrogen as a carrier gas for gas chromatography (GC) applications

·         Interlaboratory (ILS) studies using nitrogen and hydrogen with precision (focus on D3606 and D2887)

·         Preventing protonation using hydrogen as a carrier gas in GC – Mass Spectrometry (MS) applications ·         Comparing chromatography resolution in all three carrier gases

Abstract # 258 - Paper
10/12/2022 - 8:00 AM - 8:25 AM - Wisteria

A Novel Method for the Preparation and Characterization of Single Molecular Weight Polyurethanes: A Preliminary Ion Mobility and Mass Spectrometry Study

David Hercules - Vanderbilt University
Jody May - Vanderbilt University
John McLean - Vanderbilt University

Polyurethanes (PURs) are produced by reacting methylene diphenyl diisocyanate (MDI) with low MW polyols which are distributions of multiple individual diols. The PUR oligomers consist of a mixture of structural isomers at each mass in the distribution. Isomers can be studied by using monodisperse, polyols. This approach becomes intractable for larger MW polyols. We demonstrate a straightforward synthesis approach for generating PUR oligomer distributions with unique numbers of polyol attachments. Four polyols (PEG, PPG, PTHF, and PBA) were reacted with phenyl isocyanante (PhNCO) to produce distributions of PUR oligomers exhibiting unique numbers of polyol attachments. Structural characterization by Ion mobility and high resolution mass spectrometry confirmed these PUR oligomers are monodisperse and MS/MS results indicated the products follow known fragmentation mechanisms.

Abstract # 259 - Paper
10/12/2022 - 8:25 AM - 8:45 AM - Wisteria

Multidimensional Mass Spectrometry of Polymeric Materials

Chrys Wesdemiotis - The University of Akron

Progress in science and engineering relies increasingly on synthetic materials with well-defined structures, optimized to perform specific biomedical, technological, consumer, and environmental applications. Mass Spectrometry (MS) using matrix-assisted laser desorption/ionization (MALDI) and/or electrospray ionization (ESI) provides a powerful and versatile tool for the molecular characterization of such compounds as well as for imaging the molecular composition and defects of solid polymer surfaces. The dispersive nature, high mass resolution, and unparalleled sensitivity of MS permit the conclusive and confident elucidation of molecular weight (MW), functionality, and end group distributions and are particularly suitable for monitoring reactions that change the mass. This information required for both structural elucidation as well as the determination of polymerization mechanisms. Complex mixtures and multicomponent blends can be simplified with multidimensional approaches, involving in-line separation by polarity, using liquid chromatography (LC), and/or by ion size and shape, using ion mobility (IM) spectrometry. Meanwhile, large macromolecules and crosslinked networks can be made analyzable by mild thermal degradation that predictably breaks weak bonds while preserving connectivity and functionality. Conversely, mass spectrometry imaging (MSI) techniques with solvent-free MALDI can be utilized to determine the molecular composition and defects in the top molecular layer of synthetic polymer surfaces (

Abstract # 260 - Paper
10/12/2022 - 10:05 AM - 10:25 AM - Wisteria

Polymer Analysis on a Next-Generation Quadrupole Time-of-Flight Mass Spectrometer with Multi-Reflectron Time-of-Flight Technology

Bryan Katzenmeyer - Waters Corporation

This presentation will introduce the SELECT SERIES MRT mass spectrometer by Waters Corporation and how it can be applied to polymer MS analysis using both matrix-assisted laser desorption/ionization (MALDI) and electrospray ionization (ESI). The benefit that high-resolution mass spectrometry (HRMS) provides for polymer characterization is the ability to make accurate mass measurements of monomers, oligomers, and end-groups that aid primary structure elucidation and confirmation. Significant advancements in time-of-flight (ToF) MS were recently introduced in the SELECT SERIESTM MRT, a next-generation quadrupole time-of-flight (QToF) mass spectrometer. The SELECT SERIES MRT is based upon multi-reflecting time-of-flight (MRT) technology.

Abstract # 261 - Paper
10/11/2022 - 8:20 AM - 8:45 AM - Rose

The Analysis of Petroleum Samples Measured by Using GCxGC-HRTOFMS

A John Dane - JEOL USA, Inc.

In this work, a high-resolution time-of-flight mass spectrometer (HRTOFMS) equipped with a thermal modulator GCxGC system was used to analyze petroleum samples by using an electron ionization/field ionization/field desorption (EI/FI/FD) combination ion source.  Additionally, the GC-MS interface was modified to increase the temperature in this region so that higher boiling point compounds are able to be analyzed by the GCxGC-HRTOFMS system.  The results for this work will be presented.

Abstract # 262 - Paper
10/12/2022 - 8:45 AM - 9:05 AM - Wisteria

Comprehensive Two-dimensional Liquid Chromatography Coupled with Mass Spectrometry for Analysis of Complex Industrial Polymeric Materials

Peilin Yang - Dow Chemical

Synthetic polymers are widely used in our daily life.  As the world demands more sustainable, more affordable and higher-performance industrial and consumer products, there is a strong need to develop new polymeric materials that are biodegradable or derived from renewable raw materials.  Higher degree of chemical heterogeneity or presence of more polymeric impurities are among the many challenges in developing more sustainable materials.  In this presentation, we will discuss how comprehensive two-dimensional liquid chromatography coupled with mass spectrometry (LCxLC-MS) can provide new insights in the understanding of complex industrial polymeric materials at a molecular structure level. 

Abstract # 264 - Seminar
10/12/2022 - 10:25 AM - 10:55 AM - Wisteria

Application Advantages of a HR-ARRAY ICP-OES for The Trace Analysis of Silicon in LIGHT Naphtha samples

Jessica Gantt - Analytik Jena

Silicon is known to affect the performance and reduce the lifetime of hydrotreatment catalysts. Monitoring potentially silicon impurities in incoming goods, process intermediates and final products is of great importance to refineries. Total silicon content can be measured directly by ICP-OES, but the direct analysis of organic matrices is still challenging for ICP techniques. In this study, we present the application advantages for trace analysis in light naphtha samples, originating from an ICP high-resolution (HR) optics, intelligent torch design and high plasma robustness. Additionally, the benefits powerful software tools for background correction and spectral interferences are demonstrated.

Abstract # 265 - Seminar
10/12/2022 - 10:55 AM - 11:25 AM - Wisteria

A Next Generation of Microwave Sample Preparation

Bob Lockerman - CEM

The CEM BLADE Microwave Digestion System is the fastest and easiest to use system available.   It incorporates several unique features including an autosampler to load and unload samples into and out of the microwave cavity.   A simple snap on cap eliminates vessel assembly and a one of a kind camera option that allows technicians to watch their sample digest in real time.   We will provide data on how the BLADE can be used to digest a variety of oils, polymers and other samples while providing an enhanced work flow to your laboratory to help lower your cost per test.

Abstract # 266 - Seminar
10/12/2022 - 12:25 PM - 12:55 PM - Wisteria

Dedicated, High-Performance Sample Introduction Systems (HP-SIS) for ICP-OES

Randy Mercurio - Glass Expansion

The standard sample introduction system (SIS) of your ICP determines many factors, including detection limits, precision, different matrix tolerances and cost. ICP performance can often be improved by careful choice of torch, spray chamber and nebulizer components, taking into account the type of samples that will be analyzed. In this presentation we will highlight Glass Expansion’s new line of High Performance Sample Introduction Systems (HP-SIS) for the Thermo Fisher Scientific® PRO Radial and Duo ICP-OES. This presentation will help you learn how to make the right choice to get the best results and reduce operating costs, while minimizing downtime.

Abstract # 267 - Seminar
10/12/2022 - 2:00 PM - 2:30 PM - Wisteria

Design and Performance Review of Innovative Microwave Inductively Coupled Atmospheric Plasma – Optical Emission Spectroscopy (MICAP-OESTM-1000) Utilized in Determination of Elements in Used and CRM Lubricating Oils Diluted with Low Odor Kerosene.

Christine Rivera - Radom

MICAP-OES 1000 plasma operates on industrial grade (99.998%) nitrogen and 1000 W power. The technology to create the stable plasma is called Cerawave™ which replaces the traditional electric water-cooled coil. MICAP-OES 1000 was utilized to determine elements in used and CRM Lubrication oils prepared with simple dilution with low odor kerosene. The method optimization included evaluation of Glass Expansion MicroMist 0.2 mL/min and 0.4 mL/min nebulizer. Method performance will be presented including stability, LOD, accuracy and precision.

Abstract # 268 - Seminar
10/12/2022 - 2:30 PM - 3:00 PM - Wisteria

Oil Field Waters using a new plasma interface (DSOI) for ICP-OES analysis with a focus on P & Cl

Dion Tsourides - SPECTRO Analytical Instruments

The ability to measure Phosphorus and Chlorine is critical in Oil Field Waters. Traditionally it required multiple analytical techniques and/or multiple samples preparations. This presentation will discuss the advances in plasma viewing using a Dual Side On Interface which eliminates the need for multiple analysis of the same sample while simplifying the process. Cost and maintenance savings using this spectrometer system is typically >$5000 per year.

Abstract # 269 - User Group
10/12/2022 - 9:45 AM - 10:15 AM - Floral Hall A1

Hands on experience with the Agilent 8890 GC System

Jamie Wetuski - Agilent Technologies

Learn more about Agilent GC’s on board intelligence and how it can keep your lab on track. Scheduled and self-guided maintenance offers step-by-step instructions on common maintenance procedures such as changing the septa or gold seal. New Self Aware GC features allow for on board diagnostics and troubleshooting.

Come find out how the 8890 GC can improve your lab’s workflow with this hands on experience.

Abstract # 270 - Seminar
10/12/2022 - 3:00 PM - 3:30 PM - Wisteria

Let Robots Do Robot Work

Jacob Smith - CETAC

​A worldwide leader for over 30 years in sample introduction, sample preparation/dilution, and overall sample handling equipment for elemental analysis. Teledyne CETAC Technologies provides a comprehensive range of product based solutions for the analysis of elements in samples ranging from drinking water and used and new oils formulation, to high purity acids and radioactive waste.  ​Our spectroscopy and automation groups develop, manufacture and market a family of products and services for c​​​​ustomers around the world, for use in every industry where rapid and accurate determination of trace element concentrations is required.

Abstract # 271 - Paper
10/11/2022 - 1:45 PM - 2:05 PM - Wisteria

Water Determination in Liquefied Petroleum Gas using GC-UV LUMAâ„¢ and Ionic Liquid Column using hydrogen as carrier gas.

Ryan Schonert - VUV Analytics, Inc.

Water in petrochemical and refinery streams can cause problems for processors. Freezing of pipe lines and valves and also 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 Karl Fischer analysis, the GC water analyzer does not suffer from the adverse effects of the petroleum matrix which can skew the KF results. GC methods can bypass the undesirable chemical interference that would otherwise be present like “Sulfur interaction” and acetone. The use of the LUMA™ VUV detector and Supelco’s water analysis column “Watercol” are combined to separate and measure the water in a propane, propylene and butane streams. The VUV LUMA detector provides sensitive and accurate results using hydrogen as carrier gas. Measurements can be made down to water levels of less than 1 ppm.

Abstract # 272 - Paper
10/12/2022 - 11:25 AM - 11:50 AM - Tulip

Analyzing Vapors over Soils Using a Microfluidic Devices and Automated Thermal Desorption (ATD)

Chris Goss - InnotechAlberta
Simone Levy - InnoTech Alberta, Alberta Innovates
Rafal Gieleciak - Natural Resources Canada, CanmetENERGY
Lee Marotta - PerkinElmer Inc.

Determination of hydrocarbon (HC) type distribution in petroleum fluids is generally done with data from two gas chromatographs (GC); one with a flame ionization detector (FID) and one with a mass spectrometer (MS). The resulting GC-MS data is then taken through calculations based on the Robinson whole oil method to determine hydrocarbon type composition in each fraction. The method reports four saturated hydrocarbon types, twelve aromatic HC types, three tiophenic and six unidentified aromatic groups and does not require a prior separation of a sample into saturates and aromatics fractions. Moreover, the above method was applied to provide the distribution of individual HC types in function of carbon atom number defined by Simulated Distillation (SimDis) in the region of interest.

The challenge was to get a hydrocarbon breakdown on volatiles in air to attain a flux rate. Initially, the maximum concentration at steady state was determined by sampling onto two sets of thermal desorption sorbent tubes one after the other and analyzed in separate runs. The flux rate experiment was not measured in a constant state, but in a changing state. Therefore, the requirement was to sample one tube and analyze it by FID and MS detectors at the same time. To accomplish this, a microfluidic devise was employed.

The method, thermal desorption and microfluidic device developments will be discussed.