Analysis of Permanent Gases: More Challenging Than You Might Think

Permanent gases such as carbon monoxide, CO2, O2, N2, and methane are common in refinery gases, natural gas, fuel cell gases, and many other industrial processes. Permanent gas analysis finds wide application in the fields of petrochemical, chemical, and energy industries.

On the surface, this would appear to be a simple separation—however, there are several challenges related to the analysis of permanent gases. This webinar will discuss typical techniques for resolving and detecting permanent gases, including carbon dioxide and hydrogen. Other topics will include cryogenic techniques, column isolation, and the use of the Agilent J&W Select Permanent Gases/CO2 GC column.

 

Speaker

Mark Sinnott
Application Engineer
Agilent Technologies, Inc.

Mark Sinnott works for Agilent Technologies as a Technical Support Engineer in the Consumables and Supplies Division (CSD). In his position at Agilent, Mark performs technical support and applications assistance to gas chromatographers worldwide. He has more than 22 years of experience in gas chromatography, including environmental analysis of compounds in air, soil and water matrices, including dissolved gas analysis for the electrical industry. Mark holds a Master’s Degree in Chemistry from California State University, Sacramento, and currently resides in Twin Falls Idaho.

 

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Making Better Connections in GC and GC/MS Systems

This presentation will cover products from Agilent that make GC connections more robust by utilising new technologies that makes connections easier, leak free and more inert for any application.

Topics covered include: Self Tightening Stainless Column Nuts and ferrules, Press Fits, UltiMetal Plus and Stainless Steel Capillary Tubing, Ferrule Pre-swaging installation tool and MS interface installation tool, among others.

Mark Sinnott
Application Engineer
Agilent Technologies, Inc.

Mark Sinnott works for Agilent Technologies as a Technical Support Engineer in the Consumables and Supplies Division (CSD). In his position at Agilent, Mark performs technical support and applications assistance to gas chromatographers worldwide. He has more than 22 years of experience in gas chromatography, including environmental analysis of compounds in air, soil and water matrices, including dissolved gas analysis for the electrical industry. Mark holds a Master’s Degree in Chemistry from California State University, Sacramento, and currently resides in Twin Falls Idaho.

 

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Become a Better Chromatographer

Whether you are new to practicing GC chromatography, or would like a refresher, the installation and care of your GC column is of the utmost importance.

Join us as we discuss proper column installation and handling for all Agilent GCs including the Intuvo 9000. We will also address the common modes of column degradation and some of the misconceptions that people have concerning column degradation. Lastly, we will discuss ways that you can protect and maintain your column’s lifetime and performance while minimising instrument downtime.

 

Mark Sinnott
Application Engineer
Agilent Technologies, Inc.

 

Mark Sinnott works for Agilent Technologies as a Technical Support Engineer in the Consumables and Supplies Division (CSD) at the capillary column manufacturing facility (the “J&W Scientific” location). In his position at Agilent, Mark performs technical support and applications assistance to gas chromatographers worldwide. He has more than 22 years of experience in gas chromatography, including environmental analysis of compounds in air, soil and water matrices, including dissolved gas analysis for the electrical industry. Mark holds a Master’s Degree in Chemistry from California State University, Sacramento, and currently resides in Sacramento.

 

Ryan Birney
Application Engineer
Agilent Technologies, Inc.

 

In Ryan’s current role at Agilent, he provides application assistance and technical support for GC and Spectroscopy. He has been supporting Agilent in technical and sales roles for the past seven years. Ryan came to Agilent from industry, and has an BS degree in Biochemistry.

 

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Residual Solvent Analysis of Pharmaceutical Products

Organic solvents constitute a major fraction in the synthesis of pharmaceutical products. The manufacturing process for active pharmaceutical ingredients (APIs) may contribute to residual solvents remaining in the final product. Producers need to monitor and control the levels of residual solvents for several reasons—including safety, effect on crystalline form, solubility, bio-availability, and stability.

Therefore, all products must be tested to assess whether the solvents used during the manufacturing processes are within the accepted limits. Quality assurance laboratories routinely use the United States Pharmacopeia (USP) Method <467>.

 

Procedures for identification and quantification

The USP <467> monograph specifies the different classes of solvents per their toxicity, sets the concentration limits according to their health hazard, and describes the assay procedure for the solvents. A complete list of all the solvents that may be used in manufacturing processes is not mentioned under these classes. Therefore, the final products should be screened according to the solvents used during their specific manufacturing process.

The method is composed of three analytical procedures for identification and quantification.

  • Procedure A: Identification and limit testing. Uses a G43 phase (624-type column).
  • Procedure B: Confirms whether or not an identified solvent is above the regulated limits. Uses a G16 phase (WAX-type column).
  • Procedure C: Quantitative test using a G43 phase or G16 phase, depending on which produced fewer coelutions.

 

USP <467> analytical flowchart for residual solvent analysis.

 

Columns for excellent performance

Agilent J&W DB-Select 624 UI columns have shown excellent performance for residual solvent analysis according to USP <467> Procedure A. Repeatability was generally better than 2.5% RSD for Class 1, Class 2A, and Class 2B solvents. Once a residual solvent was identified above the permitted daily exposure (PDE) limit, Procedure B is performed to confirm analyte identity. The Agilent J&W DB-WAX UI GC column has been successfully used as a confirmation column, because it yields an alternate selectivity compared to that of a G43 column.

Agilent J&W DB-Select 624 UI columns

 

Recommended instruments

For this method, Chemetrix can recommend state-of-the-art analytical instruments. With best-in-class technology and powerful software, the Agilent 7697A headspace sampler is packed with the latest productivity-boosting features.  It’s unique sampling design allows you to use hydrogen as a carrier gas, delivering optimal chromatography and helping to future-proof your lab.

Agilent 7697A Headspace Sampler

 

Based on the Agilent Intuvo 9000 GC system, Agilent Residual Solvent Analyzers are factory pretested and preconfigured to deliver results, fast, while saving precious startup time. What’s more, their analytical precision exceeds USP method requirements for the three classes of residual solvents. It’s chemically tested to ensure optimal analysis of class 1 and class 2A/B solvents and labs can begin system calibration and validation immediately following installation.

Agilent Intuvo 9000 GC

 

A critical process

Residual Solvent Analysis is a must in any manufacturing environment where solvents form part of the production process. Because this process is so critical, using the correct instruments suited for the lab requirements can save time and boost accuracy.

 

Quality control at the heart of it all

At every stage of the quality control process, Chemetrix can assist labs with full end-to-end solutions for your residual solvent analysis. Our team of qualified professionals can share a comprehensive portfolio of solutions, including different instrument models, software and consumables, that work together to provide accurate and reproducible results.

 

Looking for more information on Residual Solvent Analyis? Watch our webinar >

 

Analytical Strategies for USP Residual Solvents Analysis

In this presentation, we will present the relevant GC/FID and GC/FID/MS based analytical strategies to confidently detect and quantify Class 1, 2, and 3 as well as unknown solvents in drug products. Learn how taking advantage of dual channel configuration and Agilent’s Smart, Connected, and Self-Aware systems can help you successfully meet your requirements for residual solvent analysis and ensure your testing is right first time and every time.

 

What will you learn

  • Understand what residual solvent impurities are and why it’s important to characterise and quantify them, even when present in trace amounts
  • Understand the current regulatory guidelines for residual solvent analysis in drug substance and product
  • Learn about the approaches for the confident identification and quantification of residual solvents

 

Who should attend this webinar

  • Laboratory managers
  • Chromatographers
  • Analytical chemists and scientists
  • New product developers
  • Pharma quality control managers

 

Ian Eisele
Applications Chemist,
Gas Phase Separation Division,
Agilent Technologies

 

Youjuan Zhang
Applications Chemist,
Gas Phase Separation Division,
Agilent Technologies

 

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Optimised Analysis of SVOCs with EPA 8270E

This webinar will overview a sensitive method used to analyse semivolatile organic compounds (SVOCs) on an Agilent 7000E Gas Chromatograph/Triple Quadrupole (GC/TQ) Mass Spectrometer. The utilization of GC/TQ instrumentation for analysis of SVOCs offers significant advantages:

  • Excellent selectivity afforded by Multiple Reaction Monitoring (MRM) mode results in faster batch review and increased confidence due to the elimination of matrix interferences often present when using GC/MS acquisition modes; and
  • Better sensitivity enables smaller extraction volumes which improves sustainability, reduces waste, and decreases costs associated with sample preparation, solvent usage, and waste disposal.
  • Key analytical techniques which facilitated this work will be discussed.
  • Manufacturer’s recommended tune protocol for mass accuracy and resolution checks in accordance with US EPA Method 8270E will also be discussed.

 

Rachael Ciotti
GC/MS Application Specialist
Agilent Technologies, Inc.

 

Rachael Ciotti is a GCMS Application Specialist at Agilent Technologies in Wilmington, DE. Previously, she was a Field Service Engineer specializing in installing, maintaining, and repairing Agilent GC and GC/MS systems. Prior to joining Agilent, Rachael worked at DuPont as an analytical chemist responsible for GC and GC/MS method development and transfer to manufacturing labs. She holds a Bachelor of Arts in Mathematics from Rutgers University.

 

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1,4-Dioxane in Consumer Products

1,4-Dioxane is an industrial chemical contaminant that is of concern even at trace levels in consumer products. Government jurisdictions are beginning to regulate the amount of 1,4-dioxane allowed in consumer products globally. It has already been banned and deemed unsafe in cosmetics in Canada, and it is a regulated substance in Europe. The allowable concentrations in the United States are expected to vary from state to state, typically at part per billion to low part per million levels. There have been several methods developed to test for 1,4-dioxane, but none of these methods are adequate to detect 1,4-dioxane in consumer products with complex mixtures and solutions.  A method for the high-sensitivity detection of 1-4-Dioxane was developed on the Agilent 8890B/7000 GC/QQQ triple quadrupole in Electron Ionization (EI) mode.  The extraction was performed using an Agilent PAL3 autosampler with solid phase microextraction (SPME) tool. The GC was configured with a 30 m DB-8270D column and a 1 m deactivated fused silica column using a purged ultimate union. The advantage of using a tandem quadrupole mass spectrometer is that a selective precursor to product ion transition is generated, minimizing interferences. Analysis time was less than 15 minutes. Calibration curves using 9 levels from 0.1 ng/g (ppb) to 400.0 ng/g (ppb) in multiple reaction monitoring (MRM) Electron Ionization with an R2 value of 0.999.  Low detection limits, necessary for these pernicious compounds, were also achieved.

 

 What you will learn

•    The application of the Evosep One chromatography system to high-throughput analysis of large cohorts.
•    How there is a growing demand for high throughput and standardized workflows to allow  the  analysis of increasingly large cohorts of samples for proteomic research
•    How high sensitivity is achieved for the accurate measurement of low abundant biomarkers
•    How the Evotip was designed to improve efficiency and recovery associated with sample purification and loading ahead of MS analysis.

 

Ron Honnold
Application Scientist
Agilent Technologies, Inc.

Ron Honnold, Ph.D. is an Applications Scientist in the Life Sciences and Applied Markets Group (LSAG) at Agilent Technologies; Santa Clara, CA. Ron is an experienced analytical chemist and mass spectrometrist with more than 30 years of experience using state-of-the-art analytical systems. Currently he is responsible for applications and methods development related to GC-MS products, particularly for single quadrupole (GC/MS), triple quadrupole (GC-MS/MS), and quadrupole time of flight (GC-QTOF). Ron is also a member of the Agilent Cannabis Task Group focusing on pesticides, terpenes, and residual solvents.

 

Simon Jones
GC Applications Engineer/Scientist
Agilent Technologies, Inc.

Simon Jones has over 23 years of GC experience. For the last 15 years, he has been with Agilent as a GC applications engineer/scientist based out of the GC column manufacturing facility in Folsom California. In his roles he has assisted with application development, troubleshooting chromatographic issues, and assisting with instrument configurations. Prior to joining Agilent in 2005, he worked in an analytical lab for the power industry, developing and optimizing testing methodologies for insulating fluids and materials in transformers.

 

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Gas Chromatography

Our Gas chromatography (GC) systems combine the renowned Agilent robustness with innovative technology and integrated instrument intelligence to offer labs and operators predictive technologies aimed at preventing common GC problems before they occur. We offer the broadest range of GC solutions, custom for each customer’s application.

 

Fundamentals

Learn about gas chromatographs and their main components, as well as the basics of GC separation and the common industries where GCs are used.

 

Fundamentals of Gas Chromatography (GC) – Part 1

Learn about gas chromatographs and their main components, as well as the basics of GC separation and the common industries where GCs are used.

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Fundamentals of Gas Chromatography (GC) – Part 2

Primary Components of a GC System and Steps for a GC Analysis

Fundamentals of Gas Chromatography (GC) – Part 3

Sample Injection, Separation and Detection

Fundamentals of Gas Chromatography (GC) – Part 4

Fundamentals of GC Columns