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Monitoring Gasification with a Mass Spec Gas Analyzer

Monitoring Gasification with a Mass Spec Gas Analyzer

Research in the field of biomass gasification is increasingly important as industry continues to find new uses for syngas. At the Energy & Environmental Research Center (EERC) an Extrel MAX300-RTG process mass spectrometer was used to monitor the exit stream of a Fluid Bed Gasifier. The quadrupole mass spectrometer provided fast, quantitative analysis of the syngas composition.

Over the last several years, concern about the economic and environmental impact of traditional fossil fuel combustion and petrochemicals has led to a search for viable alternatives with gasification emerging as a powerful technique for generating fuel and hydrocarbons. The gasification process makes use of materials such as coal, biomass, and waste to produce synthesis gas, or syngas. Syngas is a combustible mixture of hydrogen, carbon monoxide and carbon dioxide that generally contains a small amount of methane and some trace contaminants. Syngas is used as a fuel source to generate power and heat, or converted into products like hydrogen, for use in fuel cells or fertilizer generation, or liquid fuels via a Fischer-Tropsch reaction.

Gasification and chemical processes utilizing syngas rely upon the ability to obtain information about the composition of the gas stream exiting the reactor. The MAX300-RTG is a 7th generation process mass spectrometer capable of performing quantitative analysis on a wide variety of compounds at concentrations ranging from 100% down to 10 ppb. The 19 mm quadrupole mass filter used by the system allows for high analytical repeatability and long-term stability.

The MAX300-RTG demonstrated that it has the flexibility to quickly characterize and quantify syngas mixtures. It has the sensitivity to detect trace components at ppm levels and below, and the speed to perform each measurement in under 0.4 seconds. The ability to analyze the complete array of syngas components exiting the gasifier, from 100% down to ppm levels, makes the MAX300-RTG an instrument capable of replacing complicated analysis systems involving multiple devices and technologies. The speed of the mass spectrometer means that the MAX300-RTG can be automated to monitor gas composition at several sample points, delivering a complete set of concentrations at 20 seconds per point.

At the EERC, additional sampling at the ports downstream of the reactor could yield important insight into the operation and efficiency of the fixed beds, or be used to analyze hydrogen membrane separation, or a Fischer-Tropsch product. The speed and flexibility of the MAX300-IG, combined with the capability to run 24/7 in rugged and hazardous industrial environments, make it ideal for monitoring production scale gasification and any associated chemical processes downstream. At large facilities that utilize syngas, like ammonia plants, the MAX300-RTG and its predecessors have set the standard for analyzer automation and process control over the last several decades.

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Thermogravimetric Analysis/Mass Spectrometry (TGA-MS)

Thermogravimetric Analysis/Mass Spectrometry (TGA-MS)

An Extrel MAX300-EGA was coupled with a NETZSCH TG 209 F1 Libra to Perform Evolved Gas Analysis

The heated transfer line of the MAX300-EGA™, a quadrupole mass spectrometer designed for evolved gas analysis, was connected to the off-gas port of a NETZSCH® TG 209 F1 Libra® thermobalance. A variety of samples were analyzed and the combination of the two technologies allowed for simultaneous thermal characterization and quantitative analysis of the compounds in the furnace exhaust.

Thermogravimetric analysis (TGA) is a powerful technique that has been used for many years to characterize solid and liquid samples. The mass of the sample material is monitored while it is heated. By using a high precision balance and carefully controlling the heating process, researchers are able to plot mass loss as a function of temperature. TGA is widely used in the study of polymers, pharmaceuticals and petrochemicals to determine degradation temperatures, characterize thermal decomposition, and monitor solvent and moisture content.

Additional information about sample composition and thermal behavior can be obtained by analyzing the gases that leave the material as it is heated. This allows the researcher to determine not only the temperature at which a mass loss occurs, but also the molecular structures involved. Evolved Gas Analysis (EGA) is commonly carried out via a variety of analytical techniques, but in all cases the integrity of the gas stream must be protected. It must be kept hot and moved quickly to the gas analyzer to prevent condensation and chemical interactions.

The NETZSCH TG 209 F1 Libra is a vacuum tight TGA, making it ideal for connecting to a mass spectrometer. The Libra is equipped with an automatic sample changer and can reach temperatures up to 1100°C. It measures sample mass to a resolution of 0.1 μg. The Libra’s heated adapter was connected to the transfer line of the Extrel MAX300-EGA. The interface is differentially pumped for rapid clearing and heated to 200°C to prevent condensation; it provides a low volume, chemically inert sample path from the TGA all the way into the mass spectrometer’s ionizer.

The MAX300-EGA is a quadrupole mass spectrometer optimized for evolved gas analysis in a laboratory setting. It is capable of scanning from 1-500 amu and features the Extrel 19 mm mass filter for high analytical repeatability and long-term stability. The Questor5 software allows the system to perform qualitative analysis for sample characterization, or quantitative analysis, measuring concentrations from 100% down to 10 ppb. In addition to the transfer line, a MAX300-EGA is equipped to import a start-of-heating signal from the TGA and can be configured to perform calculations and trend data or output the data for viewing and manipulation on a different platform.

Polystyrene Decomposition: Detection of High-Mass Fragments

The furnace of the Libra was loaded with 0.94 mg of polystyrene and heated to over 600°C. The breakdown of the sample was monitored to determine the MAX300’s sensitivity to the small signals generated by high-mass hydrocarbons in the off-gas. Although the TGA records the decomposition of the polystyrene as a single weight loss beginning at 290°C, the MAX300 is able to show that the evolution of several compounds has occurred.

It is generally difficult to keep larger molecules from dropping out of an evolved sample once it has left the furnace, but the mass spectrum at 39.75 minutes clearly shows the presence of styrene in the off gas (Fig. 3. B), as well as the much smaller signal generated by methyl styrene.

The mass of each component in the gas was calculated for comparison to data from the TGA’s balance. Even the relatively small, 60 μg, loss that occurred as moisture left the sample was easily measured and quantified by the mass spectrometer. The MAX300 was also able to individually determine the amount of carbon monoxide and carbon dioxide that, combined, resulted in the second mass loss. While the thermal breakdown of calcium oxalate is well documented, the ability of the MAX300 to perform similar quantitative separations can be used to better understand a complex decomposition featuring the simultaneous evolution of multiple unknown compounds.

Further Applications for the MAX300-EGA

The data gathered from the effluent of the TGA 209 F1 Libra indicates that the MAX300-EGA is a powerful tool for evolved gas analysis. The sensitivity, resolution and quantitation demonstrated during the tests indicate the instrument’s potential for other evolved gas applications. In its standard configuration or equipped with the 300 or 400°C transfer line upgrades, the MAX300-EGA could be used to quantify solvent loss in a pharmaceutical sample, detect trace VOCs, or monitor the gas exiting a microreactor.

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Monitoring Gasification with a Mass Spec Gas Analyzer

Monitoring Gasification with a Mass Spec Gas Analyzer

Research in the field of biomass gasification is increasingly important as industry continues to find new uses for syngas. At the Energy & Environmental Research Center (EERC) an Extrel MAX300-RTG process mass spectrometer was used to monitor the exit stream of a Fluid Bed Gasifier. The quadrupole mass spectrometer provided fast, quantitative analysis of the syngas composition.

Over the last several years, concern about the economic and environmental impact of traditional fossil fuel combustion and petrochemicals has led to a search for viable alternatives with gasification emerging as a powerful technique for generating fuel and hydrocarbons. The gasification process makes use of materials such as coal, biomass, and waste to produce synthesis gas, or syngas. Syngas is a combustible mixture of hydrogen, carbon monoxide and carbon dioxide that generally contains a small amount of methane and some trace contaminants. Syngas is used as a fuel source to generate power and heat, or converted into products like hydrogen, for use in fuel cells or fertilizer generation, or liquid fuels via a Fischer-Tropsch reaction.

Gasification and chemical processes utilizing syngas rely upon the ability to obtain information about the composition of the gas stream exiting the reactor. The MAX300-RTG is a 7th generation process mass spectrometer capable of performing quantitative analysis on a wide variety of compounds at concentrations ranging from 100% down to 10 ppb. The 19 mm quadrupole mass filter used by the system allows for high analytical repeatability and long-term stability.

The MAX300-RTG demonstrated that it has the flexibility to quickly characterize and quantify syngas mixtures. It has the sensitivity to detect trace components at ppm levels and below, and the speed to perform each measurement in under 0.4 seconds. The ability to analyze the complete array of syngas components exiting the gasifier, from 100% down to ppm levels, makes the MAX300-RTG an instrument capable of replacing complicated analysis systems involving multiple devices and technologies. The speed of the mass spectrometer means that the MAX300-RTG can be automated to monitor gas composition at several sample points, delivering a complete set of concentrations at 20 seconds per point.

At the EERC, additional sampling at the ports downstream of the reactor could yield important insight into the operation and efficiency of the fixed beds, or be used to analyze hydrogen membrane separation, or a Fischer-Tropsch product. The speed and flexibility of the MAX300-IG, combined with the capability to run 24/7 in rugged and hazardous industrial environments, make it ideal for monitoring production scale gasification and any associated chemical processes downstream. At large facilities that utilize syngas, like ammonia plants, the MAX300-RTG and its predecessors have set the standard for analyzer automation and process control over the last several decades.

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The Importance of Oxygen Deficiency Monitors in the Workplace

The Importance of Oxygen Deficiency Monitors in the Workplace

If someone were to ask you what the major cause of gas related injuries in the workplace is, would your answer be carbon monoxide poisoning?

What about exposure to ammonia, hydrogen chloride, carbon dioxide, hydrogen sulfide, or chlorine? Even though injuries are reported because of over exposure to these gases, oxygen deficiency continues to pose the largest overall health risk. Often referred to as the “silent killer”, oxygen depleted breathing air is the cause of numerous injuries and/or deaths on an annual basis. Breathing air oxygen can be depleted because of leakage of stored or piped inert gases such as nitrogen, helium, argon, carbon dioxide, sulfur hexafluoride, etc. These gases, as well as others, are often used in laboratories, fertility clinics, heat treating facilities, cryotherapy installations, shipyards, various manufacturing processes, MRI (magnetic resonance imaging) installations, research facilities, dry ice manufacturing facilities, and nuclear magnetic resonance spectroscopy (NMR) installations to mention a few. According to a recent paper released by OSHA (Occupational Safety and Health Administration) “oxygen can even be consumed by rusting metal, stored ripening fruits, drying paint, combustion, or bacterial activities.” so it’s not just leakage of inert gases that can be problematic. Breathing air contains essentially 20.9% oxygen by volume. If oxygen levels drop to 14-16%, individuals exposed to those levels may become disoriented and confused.  When a sustained exposure to oxygen levels of less than 10% takes place, fainting, convulsions, and death may result. The first line of protection to help prevent injury and/or death is the use of an oxygen deficiency monitor(s).

In a January 2016 report by the Center for Disease Control and Prevention (CDC), entitled, “Sudden Deaths Among Oil and Gas Extraction Workers Resulting from Oxygen Deficiency and Inhalation of Hydrocarbon Gases and Vapors — United States, January 2010–March 2015” the article cited the potential dangers associated with exposure of workers to oxygen depleted atmospheres. A study conducted from 2010 to 2015, reported nine deaths attributed to   workers who were attempting to measure and record liquid hydrocarbon levels in storage tanks. Access to the liquid hydrocarbon was through “thief” hatches (closable apertures on atmospheric tanks, used for accessing the contents of the tank). When workers climbed to the tops of the tanks to open the thief hatch, they were often exposed to significantly depleted oxygen levels due to displacement of oxygen by the hydrocarbon vapors.

Another example of a potential low oxygen safety hazard is in MRI (magnetic resonance imaging) facilities where significant volumes of liquid helium are used to cool the MRI’s magnets. If an unexpected magnet quench (liquid helium boils off abruptly) the helium gas released into the MRI room can quickly displace breathing air oxygen levels creating a hazardous, life-threatening condition. For some installations, the volume of stored helium can be as much as 700,000 liters.  Few industries are immune from the risks of oxygen depletion, particularly when inert gases are in use. For this reason, it is prudent to use oxygen deficiency monitors to help protect personnel.

The above examples help to illustrate that the use of inert and/or process gases in the workplace can pose a real and severe threat to the well-being of individuals unless proper precautions are taken. Alpha Omega Instruments has been providing solutions to the safety market for over 26 years offering a comprehensive line of oxygen deficiency monitors and alarms.

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A Single-Supplier Solution For Impurity Monitoring In Fuel-Cell Hydrogen

A Single-Supplier Solution For Impurity Monitoring In Fuel-Cell Hydrogen

Global efforts to reduce the impact of harmful emissions on the environment have increasingly focused on lowering carbon emissions.  The key to meeting this challenge lies in replacing fossil fuels with alternative, renewable fuel sources, particularly to power vehicles.

Fuel cells offer a uniquely flexible solution in this market and can be used for a wide range of applications, powering systems from laptop computers to utility power stations.

The move to a hydrogen economy is widely regarded as the next step in the global transition towards a zero-emission energy sector. A hydrogen fuel cell uses chemical energy to cleanly and efficiently produce electricity; the only byproducts are water and heat. It can also be combined with electric motors to power a zero-emission vehicle.

While most hydrogen (H2) today is still produced from fossil sources, an established H2 infrastructure allows a future seamless transition to renewable and truly carbon-free H2 production. Fuel cells are also far more efficient than conventional combustion engines while offering a similar range (typically, about 500-700 km). H2 can also be refilled quickly at a fueling station, avoiding the delays of charging a battery-electric vehicle.

However, the performance of a fuel cell is dependent on the purity of the hydrogen. There are multiple impurities that can affect the fuel cell, and their presence and concentration levels depend largely upon the method used to generate the H2.

For example, most hydrogen is produced through steam methane reforming. This process can generate several contaminants ranging from methane and moisture to carbon monoxide and carbon dioxide (CO2). If H2 is created through electrolysis, splitting water into hydrogen and oxygen, then moisture and oxygen are the most common contaminants. Additionally, many impurities can come from the atmosphere, mostly nitrogen, oxygen, and moisture.

Eliminating impurities from H2 altogether is not practical. Maintaining an efficient fuel cell requires the presence of these contaminants to be limited to specific levels, set by international purity standards such as ISO 14687 or SAE J2719.

It is essential to monitor the wide range of impurities listed in the table above to prevent performance being compromised, or worse, irreparable damage to the fuel cell.  In the past, a monitoring solution for H2 purity involved a complex setup using as many as seven different analyzers from multiple providers, with no integration.

A typical arrangement requires:

  • A gas chromatograph for total sulfur and total halogenates
  • Another gas chromatograph for helium, nitrogen & argon, and methane/THC
  • An electrochemical analyzer for oxygen
  • An FTIR to measure CH2O2, CO and CO2
  • Three separate CRDSs, measuring water, ammonia, and CH2O

Process Insights provides a full portfolio of solutions for monitoring hydrogen purity throughout its supply chain, from production, through transport and storage, to fueling.  The contaminant detection limits of these instruments are ideally suited to qualify H2 for compliance with global purity standards.  The real benefit, however, lies in Process Insights’ total solution, which links products from its Extrel and Tiger Optics brands.  Only three analyzers are required, and these can be fully integrated into one single-provider system.

The components are:

The Prismatic 3 multi-species Cavity Ring-Down Spectroscopy (CRDS) analyzer allows simultaneous detection of up to four impurities with wide dynamic ranges, delivering simple, real-time, direct measurements. Highly reliable and with low maintenance requirements, the Prismatic 3 is ideal for remote operations and has a low cost of ownership.  Tiger Optics’ analyzers are used to support fuel-cell hydrogen quality control by organizations including the Korean Gas Safety Corporation (KGSC) and California’s Division of Measurement Standards and is approved by ISO.

The MAX300-LG is a compact benchtop mass spectrometer that delivers complete, real-time sample analysis from 100% concentration down to parts-per-billion (ppb) levels. It is supported by our Extrel easy-to-use Questor5 process control software, which is designed for continuous gas monitoring with automated calibrations, analysis sequences, and data outputs.

The combination of Process Insights’ Prismatic 3 analyzer and MAX300-LG mass spectrometer with a Sulfur & THC GC Analyzer to provide the remaining measurements provides a powerful solution for monitoring contaminants in fuel-cell hydrogen.

This system dramatically reduces the number of instruments required for measuring hydrogen samples and reduces the cost of manpower and operation through ease of use and low maintenance needs. It also means operators only deal with a single provider, reducing the complexity of ordering, integration, and usage.

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New Acquisition of the Process Analyzers Business from Schneider Electric

New Acquisition 

New Acquisition of the Process Analyzers Business from Schneider Electric

Greensboro, NC – June 24, 2022.  Process Insights, a Union Park Capital portfolio company, announced today the acquisition of the assets of the Process Analyzers business from Schneider Electric (“Schneider”).

Based in Upland, California, Schneider’s process analyzers deliver premium solutions to leading companies worldwide and serving a diverse universe of industries and process/laboratory applications including, but not limited to the chemical, life sciences (pharmaceuticals and biotechnology), metals, general industrials and energy markets.  Backed by over 35 years of technology innovation and industry expertise, the acquired FTIR/FT-NIR analyzers and the process mass spectrometers further expand Process Insights’ core gas and liquid-phase analysis and measurement capabilities and round out Process Insights’ online and laboratory product and technology portfolio for a one-stop, total solution strategy.

“This asset deal broadens and strengthens Process Insights’ already robust portfolio of analytical instrumentation and technology” said Monte Hammouri, CEO of Process Insights.  “The ANALECT® process and laboratory FTIR and FT-NIR analyzers address a premium market demand in spectroscopic capabilities and highly complement our Guided Wave brand of NIR and UV-VIS solutions.  The MGA™ magnetic sector mass spectrometer technology is a complementary extension of our Extrel brand of Quadrupole mass spectrometers.  With this deal, we continue our journey to strengthen our position as a leading global provider of comprehensive online process and laboratory analytical instrumentation to better serve our customers worldwide” added Hammouri.

“The completion of this transaction gives continuity to our customers who have purchased analyzers from Schneider in the past and now allows us to focus and pursue more growth opportunities in the instrumentation and measurement space, which align with the strategic priorities of our business,” said Matt Carrara, Vice President – Field Devices, Schneider Electric Systems USA, Inc.

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About Process Insights

Process Insights is a leading, global innovator and manufacturer of instruments focused on process analytics, monitoring, control, and safety.  Process Insights’ premium brands are used across a wide range of applications and end markets to ensure safe operation, increase product quality and attain higher levels of efficiency in process industries.  Process Insights offers a sophisticated suite of instruments, monitors, sensors and software that help customers make complex analytical measurements used in mission-critical applications to reduce disruptions, downtime, and lost productivity, all while managing increasing regulatory complexity, safety expectations and cost in industrial processes.  Process Insights is backed by Union Park Capital, a private equity investment firm based in Boston, MA.  For more information, visit www.process-insights.com.

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Why Controlling The Temperature of the Sample Interface Matters

WHY CONTROLLING THE TEMPERATURE OF THE SAMPLE INTERFACE MATTERS

Some applications such as nucleation reactions, polymer cross-linking or high viscosity fluids require that the temperature of the fluid be precisely controlled to ensure that the reaction proceeds as expected and passes through the flow cell. If the temperature drops, the fluid may solidify in the flow cell or the polymer chain may not be the correct length.

You Need To Consider A Temperature Controlled Flow Cell for At-Line FT-NIR Measurements

Our Guided Wave Multi-Purpose Flow Cell (MPFC) that is compatible with NIR and UV-VIS Analyzers is available with internal tubing for heating or cooling fluid. While the heat exchanged is not sufficient to impact a rapidly flowing sample, it can be used to maintain the temperature of a preconditioned sample.  A version of the MPFC, drilled to accept a heating or cooling fluid, is also available. While the heat exchanged is not sufficient to significantly impact a rapidly flowing sample, it can be used to maintain the temperature of a preconditioned sample.

The MPFC provides exceptional optical performance and is optically matched to all our Guided Wave analyzers Typically, peak transmission exceeds 50%. That means more signal, lower measurement noise translating to lower limits of detection.

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Do you know when to use a flow cell instead of an insertion probe

Do you know when to use a flow cell instead of an insertion probe?

Our Guided Wave Multi-Purpose Flow Cells (MPFC) are used whenever direct insertion probes are not appropriate and the process material does not require the added assurance of the High Safety Flow Cell. One of the primary advantages of near infrared process spectroscopy is the utilization of intrinsically safe fiber optic cables to remotely locate the probe. While direct insertion probes eliminate sample loops and sample systems and their associated problems, sometimes it is necessary to install sample loops for safety, service, and/or sample conditioning reasons. Our MPFC is a convenient, compact, rugged sample interface that is easy to install and even easier to service. The cell’s sapphire windows can be cleaned by simply removing a clean-out plug for direct access to the windows without disconnecting process lines or fiber optic cables.

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Why Use Process Analytical Spectroscopy for Real-Time Monitoring?

Why Use Process Analytical Spectroscopy for Real-Time Monitoring?

Traditionally, absorption spectroscopy has been used in laboratories to perform the precise analyses of samples. In recent years, as electronic circuitry and optical components have become more refined, a more robust portion of the electromagnetic spectrum – UV/VIS/NIR – has emerged for use in process analytical technology. No other technology matches the acquisition speed and the range of measurements returned by a fiber optic-based dispersive grating spectrometer. A comprehensive set of data that takes hours of laboratory analyses to acquire can be available in about a minute with a process spectrometer.

Process Analytical Technologies (PAT) have been field proven for almost three decades. It is typical for a Guided Wave scanning spectrometer running 24/7 to last more than 10 years with >99% uptime. The maintenance requirements for process spectrometers are also minimal in comparison to other monitoring techniques (for example, process gas chromatographs and online titrators). The return on investment and the low cost of operation makes Guided Wave analyzers a sensible and proven choice.

Near-infrared (NIR) spectroscopy is a non-destructive technique that can provide fast, accurate results of process conditions. NIR Spectroscopy is able to achieve real-time monitoring of multiple constituents in the process by illuminating the sample with light and analyzing how the light interacts with the sample.  Spectroscopy achieves this without the high maintenance costs or the extensive upkeep considerations typically associated with gas chromatography (GC). Additionally, optical technology often eliminates the costly sample systems and fast loops needed for process gas chromatography.

NOTE: GC analyses can have significant annual costs associated with routine maintenance, column degradation, and carrier gas consumption. Such continual costs can be greatly reduced by replacing it with our Guided Wave inline spectrometer-based analyzer.

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Cryogenic Gases: Dew Point

Cryogenic Gases: Dew Point Measurement

Cryogenic gases are normal atmospheric components which have been liquefied, separated and purified.

Although they may be supplied as a high-pressure gas, most are shipped to the customer in a liquid state and vaporized on site. The primary cryogenics are O2, N2, Ar, H2 and He are supplied in much smaller quantities.

Cryogenic gases are purchased for their particular properties. They may be used as an inert blanket, in a chemical reaction or as a catalyst. Due to this usage, they are sold in various degrees of purity. Moisture (H20) is obviously an impurity, although on a very small scale. Moisture levels will, typically, be in the 0-5 PPM range.

Due to the purity of the gas and cleanliness of the application, there are few problems with this application. The sensor should be in a bypass after the vaporizer and not directly in the flow. This will warm the sample and ensure that the flow past the sensor is not excessive.  Learn more on dew point measurement.

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