News from LabRulezGCMS Library - Week 33, 2026
LabRulez / AI: News from LabRulezGCMS Library - Week 33, 2026
Our Library never stops expanding. What are the most recent contributions to LabRulezGCMS Library in the week of 10th August 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 application notes by Agilent Technologies, Shimadzu and Thermo Fisher Scientific and poster by MDCW / JEOL!
1. Agilent Technologies: Fast Analysis of Phthalates
Using the Agilent 8850 GC/5977C GC/MSD with hydrogen carrier gas and midcolumn backflushing
- Application note
- Full PDF for download
Plastics are ubiquitous in the modern world and are used in thousands of applications. To tailor mechanical characteristics of plastics, such as flexibility, transparency, and durability for specific uses, esters of phthalic acid are often added to their formulation. These compounds are not covalently bound to the plastics in which they are mixed, and thus are easily released into the environment. They are present in a wide range of products including wire insulation, children's toys, packaging, pens, tubing, and more. Many countries now regulate phthalate content in a wide range of products. The analytical requirements for the analysis of phthalates vary depending on the region and products being tested, but GC/MS is usually the preferred measurement technique.
Given the potentially large number of samples that laboratories could be tasked to analyze, it would be valuable to have a fast-screening method to help prioritize samples for more in-depth analysis. It would also be helpful to have a method with higher chromatographic resolution for identity confirmation and quantitation using the same instrument hardware configuration.
This application note describes the development of both fast screening and conventional methods for the analysis of 19 common phthalates. The parameters considered for increasing the speed of the analysis included:
- Oven temperature program
- Column dimensions
- Column stationary phase
- Carrier gas
- Midcolumn postrun backflushing
Experimental
The system used in these experiments was configured to minimize potential problems with the hydrogen carrier gas in the analysis of the phthalates. The important parameters used were:
- Hydrogen gas: In-house hydrogen (99.9999% purity) with low water and oxygen specifications was used as a carrier gas.
- Pulsed splitless injection: Used to maximize the transfer of phthalates into the column.
- GC column: An Agilent J&W DB-EUPAH column, 20 m × 0.18 mm, 0.14 μm (p/n 121-9627) was used to obtain separation of the phthalates at high oven temperature ramp rates. The column was cut in the middle, and the ends were attached to an Agilent purged Ultimate union (PUU) (p/n G3186-60581) to provide backflushing. Purge gas was supplied to the PUU with a pneumatic switching device (PSD) module in the 8850 GC to control the flow.
- Inlet liner: The Agilent Ultra Inert inlet liner, low pressure drop with glass wool (p/n 5190-2295), was found to give good overall performance for the phthalates.
- MSD electron ionization (EI) source: When converting to hydrogen carrier gas, the choice of EI source hardware is an important consideration.1 For analytes that are subject to hydrogenation, the Agilent HydroInert source is strongly recommended because it is constructed from a material that greatly reduces the catalytic activity with hydrogen often seen in metals typically used in EI sources.
Results
Example: Pen cap
As an example, an old pen cap was tested to rapidly screen for the 19 targeted phthalates using an Agilent 8850 GC coupled with an Agilent 5977C GC/MSD system. The pen is shown in Figure 9. Samples were obtained by slicing pieces of the cap with a solvent-cleaned hobby knife. The slices were placed in a 2 mL vial with 1 mL of isooctane. The vial was capped with a PTFE crimp cap and vortexed vigorously for 1 minute. Approximately 50 µL of the extract was transferred to an autosampler vial containing a flat-bottomed insert. All the consumables (except the polyurethane caps) were baked overnight at 130 °C, as described in reference 2 before use.2 The vial was capped with a polyurethane snap cap and the extract was injected. This procedure is not quantitative; it is used to rapidly determine which, if any, of the 19 targets might be present and possibly warrant further testing.
The screening results indicated the presence of DEHP, DBP, DIBP, BBP, and DEP in the pen cap. Four of the five phthalates found here were also found in pen caps of different brands in reference 3. Only DEP was not reported in reference 3, as it was not a target, although it may have been present.
Conclusion
he methods described in this application provide both fast and conventional GC/MS analysis with the same hardware setup. Having both methods available allows for fast screening and/or higher resolution for confirmation in the same analysis sequence. Two key factors in achieving adequate separation of the phthalates in a short time are the exceptional oven ramping capability of the Agilent 8850 GC and the choice of the Agilent J&W DB-EUPAH column. The speed of the overall analysis is further improved with the use of midcolumn backflushing to eliminate the need for long postrun bakeout times to remove heavy matrix components.
2. MDCW / JEOL: WHAT DO WE DO WITH ALL THAT DATA? COMPLEMENTARY DATA PROCESSING METHODS FOR TWO-DIMENSIONAL GAS CHROMATOGRAPHY AND MASS SPECTROMETRY
- Poster
- Full PDF for download
Comprehensive two-dimensional gas chromatography combined with mass spectrometry generates a great deal of information. The different data analysis packages offer complementary features with different strengths, depending on the questions to be answered. A combined approach using different software systems is often needed to obtain a comprehensive view of the sample composition. This is illustrated for GCxGC-HRTOFMS analysis of coffee aromas.
The first step in data analysis is often determination of the types of compounds that are present. Although this is traditionally done by database searching, it is helpful to make use of other data, such as accurate mass measurements and retention index matching. For samples that have repeating units such as petrochemicals, polyhalogenated compounds, and polymers, soft ionization such as field desorption or photoionization is helpful, with or without chromatographic separation. In fact, measurements made without chromatographic separation can reveal compounds that are not suitable for gas chromatography. It's important to know what we're missing! Modified Kendrick Mass Defect plots can provide an overview of the compound classes present, and that information is helpful to guide the examination of the GCxGC-MS data with dedicated GCxGC software and identify the regions on the 2D chromatogram where different compound classes may be found. Chemometric analysis such as offered with SpectralWorks' AnalyzerPro XD software is a powerful approach to identifying differences between samples.
Methods
Headspace aromas from two single-varietal roasted coffee beans purchased from local coffee roasters and two blended coffees from Starbucks and Illy were analyzed by GCxGC-HRTOFMS. Coffee beans were ground to a fine espresso grind and approximately 10 grams of each freshly ground coffee were placed into a 20 mL headspace vial. Aroma compounds were sampled by using solid-phase microextraction (SPME) with a Supelco divinylbenzene/Carboxen SPME fiber.
A SepSolve INSIGHT thermal modulator was used for comprehensive two-dimensional gas chromatography with a normal-phase column set. Mass spectra were acquired with a JEOL AccuTOF GC-Alpha high-resolution time-of-flight mass spectrometer and a combination electron ionization (EI) and photoionization (PI) ion source. Molecular ions were present for most compounds in the EI data, so PI data were not acquired. A combination EI/FI (field ionization source) was also used to acquire FI data for one of the coffees.
Data analysis was carried out using several software packages: SepSolve ChromSpace for controlling the thermal modulator and visual comparison of GCxGC-MS data, SpectralWorks AnalyzerPro XD software for chemometric analysis, GC Image software for data analysis and figure creation. JEOL msFineAnalysis AI software was used for qualitative analysis. Mass Mountaineer software was also used for Kendrick Mass Defect Analysis of the summed GCxGC-FI mass spectral data (not shown – see our other poster).
Conclusions
Over 500 compounds were detected in the headspace volatiles for each coffee. Chemometric analysis revealed differences in the presence and relative abundances of the volatile compounds that contribute to the aromas. Chemical differences most likely relate to chemotaxonomic differences as well as differences in processing (roasting) methods. A compound that was uniquely abundant in the Colombian coffee was identified using all the available information: elemental compositions from accurate-mass and isotope data, retention index matching, and fragment ion coverage. The top database match was inconsistent with the elemental composition of the molecular ion. Of the database matches with the correct composition, none had a database retention index in good agreement with the measured value.
The msFineAnalysis AI structure analysis function identified a previously unreported compound that is not registered in the NIST and Wiley databases. This compound has a structure that is consistent with all measured GCxGC-HRMS data, and its structure is closely related to a well-known coffee aroma compound.
3. Shimadzu: The Analysis of Volatile Substances and Methanol in Spirit Drinks Using Nexis GC-2060
- Application note
- Full PDF for download
User benefits
- Nexis GC-2060 was validated for Commission Regulation (EC) No 2870/2000 for the official control of spirit drinks.
- Nexis GC-2060 provides excellent separation, high linearity, and low RSDs for reliable routine throughput.
- The Multi-Mode Injection Unit (MMI) demonstrated excellent performance to meet EC 2870/2000 criteria and significantly reduces maintenance-related downtime.
The analysis of volatile substances and methanol in spirit drinks is essential for regulatory compliance, quality control and verification of product authenticity. Commission Regulation (EC) No 2870/2000 establishes Community reference methods to ensure harmonized results during official controls and in disputes; gas chromatography with flame ionization detection (GC-FID) is the specified reference technique for quantifying key volatile congeners (aldehydes, higher alcohols, ethyl acetate) and methanol. This application note describes a GC-FID method for these analytes on a Shimadzu Nexis GC-2060, implemented to comply with the Regulation’s requirements and suitable for routine and official-control testing across a range of spirit drink categories.
This application note also evaluates Shimadzu Multi-Mode Injection Unit (MMI) operated in split/splitless mode to verify its performance to meet the requirements of the method.
Conclusions
In conclusion, analysis of volatile substances and methanol in spirit drinks using the Shimadzu Nexis GC-2060 produced robust chromatographic separation, an excellent linear detector response (R² ≥ 0.9994), and very good repeatability (≤ 6.0% RSD at low and ≤ 1% RSD at mid calibration points). Expected concentrations of QC standard were within ±10%, meeting the requirements of EC 2870/2000. The Shimadzu Multi-Mode Injection Unit (MMI), evaluated in split/splitless mode, delivered high injection precision and sensitivity and satisfied EC 2870/2000 criteria. Therefore, the MMI can be adopted for routine use since regular calibration, QC checks and repeatability criteria are met.
4. Thermo Fisher Scientific: Measuring destruction efficiency of greenhouse gases released by semiconductor fabrication tools
- Application note
- Full PDF for download
Modern materials processing activities involve the use of cold plasmas employing fluorinated gases as reactive species. Some of these gases have been demonstrated to exhibit deleterious environmental consequences resulting in their being labelled as greenhouse gases or GHGs. Among the list of GHGs undergoing intense review are those of fluorinated gases, such as NF3, CF4 , SF6, CH2F2 , etc. Many of these gases are either reactants or are generated as by-products of semiconductor wafer fabrication processes, such as etching and chemical vapor deposition. Therefore, semiconductor fabrication plants (SemiFabs) employ abatement tools to destroy and dilute these fluorinated gases before they reach a stack scrubber. This process assures that they will meet EPA regulations which require yearly facility-dependent GHG emission audits. European and Asian semiconductor manufacturers must meet similar regulations as well.
Problem
To ensure that the abatement process occurs efficiently, SemiFabs are required to audit selected abatement devices (one per each wafer processing tool employed) such that each device gets periodically reviewed for efficiency in destroying these GHGs before they are released to the scrubber. Since there are hundreds of abatement devices within a single SemiFab, the monitoring process must be accurate, fast (one or two hours), and able to monitor multiple fluorinated species simultaneously. Most SemiFabs utilize a series of devices to perform the necessary measurements required to calculate an overall destruction efficiency for each fluorinated species. Among the measurements required are the dilution factor (the overall ratio of the flowrate into the abatement device to that of the flowrate out of the abatement device). In most cases, this requires the use of a krypton gas tracer and a mass spectrometer (for measurement of flowrate out) in addition to an FTIR to measure a separate infrared-active gas tracer (for measurement of flowrate in). Also required is another more sensitive FTIR to measure the residual fluorinated gases which survived destructive processes within the abatement device. The result is a very bulky and cumbersome system to measure input and output flows and concentrations. What is needed is a much simpler and fully integrated measurement system capable of performing ALL these tasks.
Solution
Thermo Fisher Scientific has developed a new methodology for measuring abatement destruction efficiencies with a much simpler system. The system uses the Thermo Scientific™ MAX-iR™ FTIR Gas Analyzer with DTGS detector in conjunction with the Thermo Scientific™ Automated Sample Console (ASC-10™). The MAX-iR analyzer can monitor the entire IR spectral range (500-5000 cm-1) without the need for liquid nitrogen. The ASC-10 allows for the precise measurement of post-abatement flow by determining the dilution of a tracer infrared gas or gases; this obviates the need for a spacious and costly mass spectrometer and krypton gas utilized in the previous system.
A necessary pre-requisite to determining abatement efficiencies is accurate measurement of pre-abatement device gas(es) input. This was a challenge for conventional methods since the input gas concentration was so high that a second FTIR with a short pathlength gas cell was required to maintain infrared absorptions in a linear regime without saturating the detector. Unfortunately, this FTIR was too insensitive to measure the post-abatement (low gas concentration) side, thus requiring another FTIR with a much longer pathlength. In the new configuration, the ASC-10 is employed to maintain a precise dilution on the pre-abatement levels while allowing post-abatement effluents to be measured directly. In this way, the overall system is reduced from 2 FTIRs and a mass spectrometer to 1 FTIR and 1 ASC-10—a much simpler, less bulky, and equally capable system configuration.
Summary of conclusions
- It was demonstrated that a simpler, less bulky, single FTIRbased system can perform measurements of destruction efficiencies of fluorocarbon GHGs in SemiFab abatement devices to achieve performance comparable to multi-FTIR/ mass spectrometric systems, thus creating a faster, less costly, and easier tool to use for the customer.
- This same system also has the capability of directly monitoring the process gasses in the etch tool and reactive by-products during the plasma etch sequence.
- Further added value is offered by the MAX Acquisition Automation software by detecting and characterizing unknown features within the analyzed spectrum to provide a fuller analysis of the etch process.
