News from LabRulezGCMS Library - Week 06, 2026
LabRulez: News from LabRulezGCMS Library - Week 06, 2026
Our Library never stops expanding. What are the most recent contributions to LabRulezGCMS Library in the week of 2nd February 2026? Check out new documents from the field of the gas phase, especially GC and GC/MS techniques!
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This week we bring you technical note by Agilent Technologies and application notes by BaySpec, Metrohm and Shimadzu!
1. Agilent Technologies: What Causes GC Capillary Column Performance Degradation, and How Can I Prevent It?
- Technical note
- Full PDF for download
Thermal damage
Exceeding a column's upper temperature limit results in accelerated degradation of the stationary phase and tubing surface. This results in the premature onset of excessive column bleed, peak tailing for active compounds, and/or loss of efficiency (resolution). Fortunately, thermal damage is a slower process, and significant damage will only occur after prolonged times above the temperature limit. Thermal damage is greatly accelerated in the presence of oxygen. Overheating a column with a leak or high oxygen levels in the carrier gas results in rapid and permanent column damage. Setting the GC's maximum oven temperature at or only a few degrees above the column's temperature limit is the best way to prevent thermal damage. This prevents accidental overheating of the column.
If a column is thermally damaged, it may still be functional. Remove the column from the detector. Heat the column for 8 to 16 hours at its isothermal temperature limit. Remove 10 to 15 cm from the detector end of the column. Reinstall the column and condition as usual. The column usually does not return to its original performance; however, it is often still functional. The life of the column will be reduced after thermal damage.
Oxygen damage
Oxygen is an enemy to most capillary GC columns. While no column damage occurs at or near ambient temperatures, severe damage occurs as the column temperature increases. In general, the temperature and oxygen concentration at which significant damage occurs is lower for polar stationary phases. Constant exposure to oxygen is the problem. Momentary exposure, such as an injection of air or a very short-duration septum nut removal, is not an issue.
A leak in the carrier gas flow path (e.g., gas lines, fittings, or injector) is the most common source of oxygen exposure. As the column is heated, very rapid degradation of the stationary phase occurs. This results in the premature onset of excessive column bleed, peak tailing for active compounds, and/or loss of efficiency (resolution).
These are the same symptoms as for thermal damage. Unfortunately, by the time oxygen damage is discovered, significant column damage has already occurred. In less severe cases, the column may still be functional but at a reduced performance level. In more severe cases, the column is irreversibly damaged. Maintaining an oxygen- and leak‑free system is the best way to prevent oxygen damage. Good GC system maintenance includes periodically checking gas lines and regulators for leaks, changing the septa regularly, using high-quality carrier gases, installing and changing oxygen traps, and changing gas cylinders before they are completely empty.
Chemical damage
There are relatively few compounds that damage stationary phases. Introducing nonvolatile compounds (e.g., salts) in a column often degrades performance, but damage to the stationary phase does not occur. These residues can often be removed and performance returned by solvent-rinsing the column. Inorganic or mineral bases and acids are the primary compounds to avoid introducing into a column. The acids include hydrochloric (HCl), sulfuric (H2SO4 ), nitric (HNO3), phosphoric (H3PO4), and chromic (CrO3 ). The bases include potassium hydroxide (KOH), sodium hydroxide (NaOH), and ammonium hydroxide (NH4OH). Most of these acids and bases are not very volatile and accumulate at the front of the column. If allowed to remain, the acids or bases damage the stationary phase. This results in the premature onset of excessive column bleed, peak tailing for active compounds, and/or loss of efficiency (resolution). The symptoms are very similar to thermal and oxygen damage. HCl and NH4OH are the least harmful of the group. Both tend to follow any water that is present in the sample. If the water is not retained or only poorly retained by the column, the residence time of the HCl and NH4OH in the column is short. This tends to eliminate or minimize any damage by these compounds. Thus, if HCl or NH4OH are present in a sample, using conditions or a column with no water retention will render these compounds relatively harmless to the column.
Column contamination
Column contamination is one of the most common problems encountered in capillary GC. Unfortunately, it mimics a wide variety of problems and is often misdiagnosed as another problem. A contaminated column is usually not damaged, but it may be rendered useless.
There are two basic types of contaminants: nonvolatile and semivolatile. Nonvolatile contaminants or residues do not elute and accumulate in the column. The column becomes coated with these residues, which interfere with the proper partitioning of solutes in and out of the stationary phase. Also, the residues may interact with active solutes, resulting in peak adsorption problems (evident as peak tailing or loss of peak size). Active solutes are those containing a hydroxyl (-OH) or amine (-NH) group, and some thiols (-SH) and aldehydes. Semivolatile contaminants or residues accumulate in the column but eventually elute. Hours to days may elapse before they completely leave the column. Like nonvolatile residues, they may cause peak shape and size problems. In addition, are usually responsible for many baseline problems (instability, wander, drift, ghost peaks, etc.).
2. BaySpec: Field Explosives Detection with the Continuity™ Portable Mass Spectrometer
- Application note
- Full PDF for download
The detection and prevention of explosive materials are paramount to ensuring public safety and national security, both within the United States and globally. The persistent threat of terrorist activities, coupled with the rise of homemade explosive devices, underscores the urgent need for advanced detection technologies. According to the Global Terrorism Database, over 8,000 terrorist attacks occurred worldwide in 2020, many involving improvised explosive devices (IEDs). The ability to detect and identify explosives before they are deployed is crucial in preventing such devastating events and protecting civilian lives.
Traditional methods for explosive detection, such as laboratory-based analysis and canine units, while effective, often face limitations due to high costs, logistical complexity, and the time required for thorough analysis. These challenges are especially pronounced in dynamic environments like transportation hubs, large public gatherings, and conflict zones, where the capacity to rapidly identify explosive materials can be the difference between life and death.
In recent years, portable mass spectrometry has emerged as a groundbreaking solution for the detection of explosive substances. Unlike conventional laboratory equipment, portable mass spectrometers facilitate real-time, on-site analysis, empowering security personnel, first responders, and military units to swiftly and accurately identify explosive compounds. This technology can be deployed in a variety of settings, from airports and border crossings to battlefield environments, offering a versatile and reliable tool for enhancing security measures. As the threat of terrorism continues to evolve, integrating portable mass spectrometry into explosive detection strategies represents a significant advancement in safeguarding communities and protecting critical infrastructure.
Experimental
Instrumentation
A BaySpec Continuity™ Portable Mass Spectrometer equipped with a Swab-APCI source was used in these experiments. The ionization source was specifically designed to accommodate TSA-approved swabs. The samples on swabs were vaporized in the Swab vaporizer unit and subsequently drawn into the ionization chamber by the built-in sampling pump.
Conclusions
This study has demonstrated the exceptional capabilities of the Continuity™ Field Portable Mass Spectrometer, equipped with a Swab-APCI ionization source, in the detection and identification of explosive materials across a range of environments. Calibration curves for TNT, RDX, HMX, and PETN provided a robust quantitative assessment, confirming the ability of the system to achieve low Limits of Detection (LODs) with unparalleled sensitivity and accuracy in MS2 mode. These results underscore the instrument’s capacity to reliably identify trace levels of explosive compounds, critical in both laboratory and field settings.
The field applications conducted, including blast pit testing and sensitive site analysis at a certified explosives mixing facility, further validated the instrument’s real-world utility. The Continuity™ system successfully detected residual explosives in complex environments, proving its robustness and reliability. The detection of HMX and RDX on a variety of surfaces, even in the presence of potential interferences, emphasizes the system’s precision and effectiveness in ensuring environmental safety and contamination control.
These findings highlight the Continuity™ Portable Mass Spectrometer as an indispensable tool for security personnel, military operations, and industrial safety. Its rapid, on-site detection capabilities, combined with high sensitivity and accuracy, offer a significant advancement in the field of explosives detection. As global security challenges continue to evolve, the integration of such portable mass spectrometry technology into field operations can substantially enhance the ability to detect, mitigate, and respond to explosive threats, thereby contributing to the safety and security of both public and sensitive environments. The Continuity™ system not only meets but exceeds the rigorous demands of real-time explosives analysis, positioning it as a leading solution for ensuring public safety and national security in an increasingly complex threat landscape.
3. Metrohm: Estimation of amine value in epoxies with Raman spectroscopy
- Application note
- Full PDF for download
A complementary approach to potentiometric titration
Amine value is traditionally determined using strong acid/weak base titration following ASTM methods [3]. While precise, this approach is labor intensive and requires chemicals, sample preparation, and sufficient time for complete titration through the endpoint. In contrast, Raman spectroscopy offers a faster, more efficient alternative and enables rapid, nondestructive, and contactless analysis of hardeners with no need for sample preparation. This Application Note details the use of Raman spectroscopy to determine the AV of a hardener, with results validated through statistical comparison to conventional titration methods.
CONFIGURATION
The i-Raman NxG 785H is ideal for routine quality control and process monitoring, especially where speed, stability, and reliability are essential. It offers a balanced combination of performance and efficiency to measure Raman scattering from 100 – 2800 cm-1. Designed to support high signal throughput, this flexible system is ideal for monitoring chemical and polymer reactions, optimizing processes, and performing content uniformity testing of pharmaceutical tablets. The i-Raman NxG 785H can be easily adapted for see-through measurements even through opaque containers, adding to its versatility.
The i-Raman NxG 785H is the go-to solution for teams looking for reliable Raman analysis in challenging operational environments.
Discover why the i-Raman NxG is the perfect way to gain control of your quality control measurements:
- High-sensitivity spectrometers deliver results in seconds and can detect the faintest Raman signals
- Flexible fiber optic probe compatible with a wide array of accessories, including a vial holder, cuvette holder, immersion probe, and seethrough adapter
- Powerful SpecSuite software for easy Raman data collection in addition to quantitative model building, identification with spectral libraries, and routine analysis
- Compact and stackable to save on valuable bench space.
CONCLUSION
Raman spectroscopy serves as a rapid and reliable secondary method for estimating the AV of epoxy hardeners. Raman predictions using a calibration model based on characteristic vibrational bands showed excellent agreement with standard potentiometric titration, with deviations within ±3%. Validation with blind samples further confirmed its accuracy. While titration remains the primary method for determining AV, Raman spectroscopy offers significant advantages with its speed, simplicity, and nondestructive nature, making it well-suited for supplemental use in quality control and process monitoring of epoxy resin systems.
4. Shimadzu: What’s in Your Brew? Detecting Volatile PFAS with Headspace SPME GC/MS/MS
- Application note
- Full PDF for download
User Benefits
- Employing the highly sensitive and selective Shimadzu GCMS-TQ8040 NX triple quadrupole mass spectrometer allows for low limits of quantitation for volatile PFAS while minimizing matrix interferences.
- Using the multifunctional AOCTM-6000 Plus autosampler, the automated SPME method and simplified sample preparation help to reduce operation errorsin PFAS analysis.
- The Shimadzu HS-SPME GC/MS/MS system can quantify volatile PFAS in beer matrices with minimal sample preparation.
- HS-SPME GC/MS/MS is used as a complementary technique to LC/MS in providing a total solution for beverage safety.
PFAS, or per- and polyfluoroalkyl substances, are a group of synthetic organic chemicals that are known for their persistence, bioaccumulation, and toxicity in the environment. 1-4 The global concern surrounding PFAS pollution continues to grow, as many of their long-term effects on health and the environment are still not fully known. 1,3 Some major human exposure routes to these harmful chemicals include inhalation of contaminated dust, breathing air containing PFAS, transfer to infants through breast milk, and ingestion of contaminated food,such asseafood, drinking water, and even commercial beverages. 1,5-7
Beer is one of the most consumed beverages worldwide. It is estimated that humans consume more than 49.6 billion gallons of beer in just one year. 7 Beer can be both alcoholic and non-alcoholic and varies in flavor, color, and aroma. Its complex composition, resulting from diverse ingredients and brewing processes, presents analytical challenges for detecting trace-level contaminants. As public awareness and regulatory attention increase, there is a growing need for reliable methods to screen beer for PFAS contamination and ensure product safety. 8 Developing an effective analytical workflow for PFAS analysis in beer matrices is therefore essential to identify contaminated batches and prevent PFAS consumption. This study aims to establish a precise and accurate quantitation method to analyze volatile PFAS in beer. Given the diverse samples analyzed in this study, this method may also be applicable to other alcoholic, non-alcoholic, and carbonated beverages.
This study presents a simple approach for analyzing volatile PFAS including fluorotelomer alcohols and acrylates in beer using HeadSpace Solid Phase Microextraction-Triple Quadrupole Gas Chromatography/Mass Spectrometry (HS-SPME GC/MS/MS). This GC/MS method addresses volatile PFAS compounds that are impractical to analyze by LC/MS. The HS-SPME technique, with its minimal sample preparation procedure and fast workflow, offers additional benefitsfor volatile PFAS analysis in complex matrices.
HS-SPME allows a pre-concentration step as well as higher selectivity compared to GC/MS liquid injection, thus allowing lower detection limits. While previous PFASHS-SPME GC/MS/MS methods have been developed for simple matrices such as drinking and bottled water, 9-11 the complex composition of beer matrices requires additional isotopically labeled internal standards to effectively compensate for matrix effects.
Method
Instrumentation: The instrument system configuration for the application consisted of a Shimadzu GC/MS triple quadrupole mass spectrometer, model GCMS-TQ8040 NX, a multifunctional autosampler (AOC-6000 Plus) equipped with a SPME module and a split/spitlessinlet.
Conclusion
A simple and innovative approach was developed to measure PFAS in complex beer samples. A Shimadzu GCMS-TQ8040 NX triple quadrupole mass spectrometer, configured with an AOC6000 Plus solid-phase microextraction (SPME) unit was used for the analysis.
Method blanks showed no detectable PFAS, and the calibration curve demonstrated excellent linearity (R² ≥ 0.996). ICV and CCV recoveries were all within 70–130%, established as the method criteria. For general method performance a LCS was evaluated. The mean PFAS recovery in the LCS was 91 to 101%, while the % RSD for the analytes in these replicates ranged from 0.9 to 6.5%. LCS results met the mean % recovery and %RSD method criteria, which were established respectively at 70-130% and ≤ 20%. An isotope dilution approach was used for all compounds to achieve accurate quantitation in complex beer matrices. Overall, the mean percent recovery for the five beer samples ranged from 78 - 126% and % RSD < 8 for all compounds. The overall results satisfied the method criteria.
The workflow presented in the study offers key advantages in terms of simplicity, speed, precision, and accuracy that are critical for routine monitoring of volatile PFAS in challenging matrices.
