News from LabRulezGCMS Library - Week 24, 2025

Our Library never stops expanding. What are the most recent contributions to LabRulezGCMS Library in the week of 9th June 2025? Check out new documents from the field of the gas phase, especially GC and GC/MS techniques!

👉 SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT GCMS AND RELATED TECHNIQUES

👉 Need info about different analytical techniques? Peek into LabRulezLCMS or LabRulezICPMS libraries.

This week we bring you application notes by Agilent Technologies and Shimadzu and presentation by  University of Liege / MDCW!

1. Agilent Technologies: Indoor Air Analysis of Fluorotelomer Alcohols and Per- and Polyfluoroalkyl Substances

• Application note
• Full PDF for download

FTOHs are a subcategory of per- and polyfluoroalkyl substances (PFAS). FTOH compounds are primarily used as precursors for PFAS compounds, such as perfluorinated carboxylic acids (PFCA), including perfluorooctanoic acid (PFOA) and perfluorohexanoic acid (PFHxA). FTOH compounds are also used as raw materials in various industrial applications due to their water- and oil repellent characteristics. 

The presence of PFAS in air is an emerging concern, prompting the growth of air quality monitoring for PFAS in analytical chemistry. Existing methods like the United States Environmental Protection Agency (EPA) Other Test Method 50 (OTM-50) are used to detect volatile fluorinated compounds and short-chain PFAS compounds in air emissions from stationary sources.¹ It is suspected that indoor air monitoring for PFAS will be a future focus area due to the use of PFAS in several household and consumer products. 

Volatile PFAS concentrations in ambient and indoor air can be low, requiring large volumes of air to be sampled. Thermal desorption, where air is drawn onto sorbent-filled tubes and later analyzed using GC/MS, is an ideal technique for large volume sampling. However, large amounts of the matrix are also drawn into the tubes and can present issues with both carryover and interference with analyte signals. GC/TQ largely eliminates these interferences and background noise while adding more specificity to detection. The elimination of noise also lowers detection limits, which is critical when determining low levels of PFAS in air.

This application note introduces a thermal desorption GC/TQ method for determining FTOH in indoor air samples. The effectiveness of the analytical method is demonstrated through the successful analysis of several real-world indoor air samples.

Experimental 

Instrumentation 

The analysis of FTOH in indoor air was performed on an Agilent 8890 GC with an Agilent 7000E GC/TQ. The system was equipped with a GERSTEL TD Core System for TD sampling, which is optimized for ambient air analyses. GC and MS method parameters are detailed in Tables 1 to 3.

Results and discussion 

FTOH standards were used to generate calibration data for the four target compounds. Analytes were evaluated at concentrations between 0.075 and 15 ng/tube. For simplicity, instrument detection limits were approximated as being 10-fold lower than the lowest calibration concentration. Calibration results are shown in Table 4.

Conclusion 

This study demonstrates the utility of an Agilent 8890 GC with an Agilent 7000E GC/TQ for the analysis of FTOH compounds in indoor air samples. The GC/TQ system was equipped with a GERSTEL TD Core System, which enabled thermal desorption sampling of ambient air. This selective GC/TQ analytical method provided good reproducibility, recovery, and sensitivity. Real-world indoor air samples proved the necessity of methods like the one described in this work, as FTOH compounds were present in all samples.

2.  University of Liege / MDCW: ONE-STEP MICROWAVE-ASSISTED EXTRACTION AND DERIVATIZATION FOLLOWED BY COMPREHENSIVE TWO-DIMENSIONAL CHROMATOGRAPHY COUPLED WITH FLAME IONIZATION DETECTOR TO FAMEs ANALYSIS IN COMPLEX FOOD MATRICES

• Presentation
• Full PDF for download

A novel one-step microwave-assisted extraction and derivatization (MAED) method, combined with comprehensive two-dimensional gas chromatography with flame ionization detection (GC×GC–FID), has been developed to improve the analysis of fatty acid methyl esters (FAMEs) in complex food matrices. This innovative approach offers a rapid, energy-efficient, and environmentally friendly alternative to traditional methods, enabling simultaneous extraction and derivatization in just 15 minutes at 120 °C.

Compared to conventional procedures (AOCS Ce2b-11 and Ce2c-11), the MAED method demonstrated equivalent accuracy and reliability in quantifying saturated, monounsaturated, and polyunsaturated fatty acids. Furthermore, GC×GC–FID significantly enhances separation, reduces co-elution, and increases sensitivity, providing structured chromatograms that facilitate more detailed FAME profiling—even without the need for mass spectrometry.

The method also proves to be scalable and suitable for high-throughput applications: up to 48 samples can be processed per hour, with reduced solvent use and lower energy consumption. Notably, when analyzing complex samples such as mussels, GC×GC–FID identified over 80 FAME peaks—vastly outperforming conventional one-dimensional GC in resolution and nutritional characterization.

Overall, MAED coupled with GC×GC–FID offers a greener, faster, and more practical solution for lipid analysis in food, enabling robust automation and supporting modern nutritional and food quality assessments. This makes it an attractive tool for both academic research and industrial quality control.

3. Shimadzu: Simultaneous Analysis of 19 Organic Solvents and Additives in Lithium-Ion Battery Electrolytes Using GC-MS

• Application note
• Full PDF for download

User Benefits:

• Simultaneous analysis of 19 organic solvents and additives reduces analytical time and improves efficiency.
• This method is suitable for the characterization of commercial LIB electrolyte formulations. 

Lithium-ion batteries (LIBs) are eco-friendly, rechargeable energy storage devices that provide a sustainable alternative to fossil fuels. They are widely used to power electric vehicles and store energy generated from renewable sources, thereby reducing dependence on fossil fuels and lowering greenhouse gas emissions. As a result, LIBs play a essential role in the transition toward low-carbon and sustainable energy systems. 

The electrolytes in LIB consists of a lithium salt dissolved in a mixture of organic solvents and formulated with various functional additives. The organic solvents act as the vehicle for lithium-ion transport between electrodes, while the additives improve electrolytes stability, safety, and overall performance by enabling stable operation under various conditions. Both organic solvents and additives play an essential roles in the function and performance of LIBs. 

Accurate control of electrolytes composition is critical, as even minor impurities in the solvents or additives can result in significant safety risks and degradation of battery performance. Therefore, the analysis of electrolytes composition and its operational degradation products is essential for ensuring the safety, stability, and quality of LIBs throughout their development and production. In a previous Application News, the analysis of seven compounds used as organic solvents and additivesin LIB electrolytes using GC-FID was proposed.¹ 

In this study, an analytical method of 19 organic solvents and additives commonly used in LIBs electrolytes was developed. The analysis was carried out using the Shimadzu Nexis GC2030 gas chromatograph coupled with the QP2020NX single quadrupole mass spectrometer. The developed method was successfully applied to commercial LIB electrolyte sample.

Materials & Method 

Analytes and Analytical Conditions 

In this study, 19 target compounds mainly used as organic solvents and additives in the LIB electrolytes were selected and then analyzed for simultaneous analysis using SHIMADZU GC2030 + QP2020NX (Figure 1). All 19 standard compounds were obtained from TCI Chemical (Tokyo, Japan) and dichloromethane (DCM) was purchased from Tedia (Fairfield, OH, USA). Detailed analytical conditions of the instrument are shown in Table 1 and 2.

Results 

The retention times and selected ions listed in Table 2 were determined by analyzing individual standard solutions under optimized GC-MS conditions. For quantification, the ions exhibiting the highest intensity and selectivity were selected. The SIM chromatograms of 19 organic solvents and additives are shown in Figure 2. The calibration curves for all standard compounds are excellent linearity, with correlation coefficients (R²) greater than 0.999 (Figure 3). The developed analytical method was successfully applied to actual LIB electrolyte samples, confirming the presence and quantifying the concentrations of three organic solvents (EC, EMC, DMC) and four additives (VC, FEC, PS, SN), as summarized in Table 3.

Conclusions

In this study, a simultaneous GC-MS method was developed and validated for the quantitative analysis of 19 organic solvents and additives in LIB electrolytes. The calibration curves demonstrated excellent linearity for all target compounds. Furthermore, The method was successfully applied to actual LIB electrolyte samples. This analytical method provides a reliable approach for lithium-ion battery research and quality assessment.