Skip to main content

Author: Terri Melle-Johnson

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.

Continue reading

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.

Continue reading

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.

####

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.

Continue reading

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

Process Insights_Guided Wave MPFC – Multi-Purpose Process Flow Cell

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.

Continue reading

Glove Boxes: Sensors

Selecting an Oxygen Monitor Sensor for a Glove Box Applications

Glove boxes are used to perform manual manufacturing processes where exposure to the components may be harmful to personnel, or exposure to the room atmosphere may be harmful to the product.

Glove boxes, generally, are purged with N2, Ar or CDA to form an inert boundary. They are widely used in the semiconductor/electronic component metalworking, nuclear and crystal manufacturing industries.  Many glove box problems are unique. Gases and residual products can produce aggressive chemicals. In some instances, sensors have required bi-weekly recalibration and a 3–6-month replacement. Most glove box applications, however, are much easier with normal sensor lifetimes expected.

Sensors are normally installed directly into the box. Our preference is to mount the sensor in a sample cell on the discharge point (there is normally a continuous bleed on glove boxes) to minimize the chance of physical damage.  Learn more on oxygen monitor sensors.

Continue reading

Know the Difference Between Oxygen Monitor Sensors

KNOW THE DIFFERENCE BETWEEN OXYGEN MONITOR SENSORS

Do you know the difference between oxygen monitor sensors?  Oxygen analyzers use one of a several types of oxygen sensors.   As industrial process applications call for improved measurement accuracy and repeatability, users are demanding analyzers that require a minimum of maintenance and calibration.   There is no one universal oxygen sensor type.

AMBIENT TEMPERATURE ELECTROCHEMICAL SENSOR

  • Often referred to as a galvanic sensor, is typically a small, partially sealed, cylindrical device (1-1/4” diameter by 0.75” height) that contains two dissimilar electrodes immersed in an aqueous electrolyte, commonly potassium hydroxide.
  • Refinements in electrode materials, and enhanced electrolyte formulations, the galvanic oxygen sensor provides extended life over earlier versions and are recognized for their accuracy in both the percent and traces oxygen ranges.
  • Response times have also been improved.
  • They are easy to damage when used with samples containing acid gas species such as hydrogen sulfide, hydrogen chloride, sulfur dioxide, etc.

PARAMAGNETIC OXYGEN SENSORS

  • This is the magnetodynamic or `dumbbell’ type of design and is the predominate sensor type.
  • The paramagnetic oxygen sensor consists of a cylindrical shaped container inside of which is placed a small glass dumbbell.  The dumbbell is filled with an inert gas such as nitrogen and suspended on a taut platinum wire within a non-uniform magnetic field.
  • A precision optical system consisting of a light source, photodiode, and amplifier circuit is used to measure the degree of rotation of the dumbbell.
  • Some paramagnetic oxygen sensor designs, have an opposing current is applied to restore the dumbbell to its normal position.
  • In general, paramagnetic oxygen sensors offer very good response time characteristics and use no consumable parts, making sensor life, under normal conditions, quite good.
  • Offers excellent precision over a range of 1% to 100% oxygen.
  • They are quite delicate and sensitive to vibration and/or position.
  • Due to the loss in measurement sensitivity, in general, the paramagnetic oxygen sensor is not recommended for trace oxygen measurements.

POLAROGRAPHIC OXYGEN SENSORS

  • Often referred to as a Clark Cell [J. L. Clark (1822- 1898)].
  • This sensor, both the anode (typically silver) and cathode (typically gold) are immersed in an aqueous electrolyte of potassium chloride.
  • The electrodes are separated from the sample by a semi-permeable membrane that provides the mechanism to diffuse oxygen into the sensor.
  • The current output generated from the sensor is measured and amplified electronically to provide a percent oxygen measurement.
  • An advantage of the polarographic oxygen sensor is that while inoperative, there is no consumption of the electrode (anode).
  • Storage times are almost indefinite. Similar to the galvanic oxygen sensor, they are not position sensitive.
  • One major advantage of this sensor type is its ability to measure parts per billion levels of oxygen.
  • The sensors are position sensitive and replacement costs are quite expensive, in some cases, paralleling that of an entire analyzer of another sensor type.
  • Not recommended for applications where oxygen concentrations exceed 25%.

ZIRCONIUM OXIDE OXYGEN SENSORS

  • This sensor is referred to as the “high temperature” electrochemical sensor and is based on the Nernst principle [W. H. Nernst (1864-1941)].
  • Zirconium oxide sensors use a solid-state electrolyte typically fabricated from zirconium oxide stabilized with yttrium oxide. The zirconium oxide probe is plated on opposing sides with platinum which serves as the sensor electrodes.
  • The zirconium oxide oxygen sensor has excellent response time characteristics.
  • The same sensor can be used to measure 100% oxygen, as well as parts per billion concentrations.
  • Due to the high temperatures of operation, the life of the sensor can be shortened by on/off operation.
  • A major limitation is their unsuitability for trace oxygen measurements when reducing gases (hydrocarbons of any species, hydrogen, and carbon monoxide) are present in the sample gas. At operating temperatures of 650 degrees Centigrade, the reducing gases will react with the oxygen, consuming it prior to measurement thus producing a lower than actual oxygen reading.
  • The magnitude of the error is proportional to the concentration of reducing gas.
  • Zirconium oxide oxygen sensors are the “defacto standard” for in-situ combustion control applications.

Explore our range of oxygen safety and deficiency monitors.

Continue reading

Welcome Guided Wave

Welcome Guided Wave

Process Insights Announces Acquisition of Guided Wave Inc.

Greensboro, NC – March 1, 2022.  Process Insights, a Union Park Capital portfolio company, announced today that it has acquired Guided Wave Inc. (“Guided Wave”) from Singapore-based Advanced Holdings Ltd.  Guided Wave, based in Rancho Cordova, California will join Process Insights’ existing broad portfolio of premium brands and technologies for process analytics, monitoring and control including COSA Xentaur, Hygrocontrol, Alpha Omega Instruments, LAR Process Analysers, Tiger Optics, ATOM Instrument, Extrel CMS and MBW Calibration.

Founded in 1983, Guided Wave designs and manufactures complete analytical systems utilizing Near Infrared (“NIR”) and Ultraviolet/Visible (“UV-VIS”) spectroscopic technologies.  Guided Wave is the only process NIR company that provides a complete, optically matched NIR analytical system yielding the best throughput efficiency and long-term performance that exceed industry standards.  Guided Wave’s analytical systems are designed for continuous online process performance while providing real-time data of laboratory quality in harsh, hazardous, and demanding environments.  Guided Wave’s products and technologies are used in a wide range of applications across a multitude of markets and industries including chemicals, petrochemicals, semiconductor, pharmaceuticals, biotechnology, and healthcare (sterilization and virus deactivation).

“For more than 35 years, Guided Wave has served a variety of customers and industries worldwide with leading spectroscopic process analyzer solutions.  With our acquisition by Process Insights, additional resources will propel Guided Wave into the next decade of innovation and industry leadership”, said Susan Foulk, President of Guided Wave.  “It’s exciting to join the Process Insights team, and the team at Guided Wave looks forward to opening new pathways for growth as we continue to put our customers and their process analytical needs first”, Foulk added.

“Guided Wave is a natural fit for Process Insights.  We share many common customers, markets and applications.  This is an exciting opportunity for Process Insights to continue to expand our total differentiated solution offerings to our customers with the addition of Guided Wave’s premium NIR and UV-VIS technologies to our portfolio”, said Monte Hammouri, CEO of Process Insights.  “We have known Guided Wave, Susan and her team for many years through prior collaborations.  Bringing them into the Process Insights family takes our collaboration to that next level where we can leverage Process Insights’ global scale and operating footprints to further accelerate Guided Wave’s growth and innovation”, added Hammouri.

Continue reading