<p><strong>Our Library never stops expanding. What are the most recent contributions to LabRulezGCMS Library in the week of 24th November 2025? Check out new documents from the field of the gas phase, especially GC and GC/MS techniques!</strong></p><blockquote><p><span style="font-size:20px;">👉 </span><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library"><span style="font-size:20px;"><strong>SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT GCMS AND RELATED TECHNIQUES</strong></span></a></p></blockquote><blockquote><p><strong>👉 Need info about different analytical techniques?</strong> Peek into <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library"><strong>LabRulezLCMS</strong></a> or <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library"><strong>LabRulezICPMS</strong></a> libraries.</p></blockquote><p>This week we bring you brochure by <strong>Agilent Technologies, </strong>poster by<strong> LECO /MDCW, </strong>and application notes by <strong>Shimadzu </strong>and<strong> Thermo Fisher Scientific!</strong></p><h3><strong>1. Agilent Technologies: GC workflows for hydrogen vehicles and natural gas blending - Hydrogen Fuel Testing Solutions</strong></h3><ul><li>Brochure</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/ac_hydrogen_fuel_purity_matters_compendium_5994_8643en_agilent_8da57fb7a2.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Agilent’s <i>Hydrogen Fuel Testing Solutions</i> compendium highlights the growing importance of reliable impurity analysis as hydrogen becomes a key clean-energy fuel. Because contaminants such as moisture, sulfur compounds, ammonia, oxygen, or organics can compromise fuel-cell performance and safety, the brochure emphasizes that hydrogen purity must be monitored throughout the entire supply chain—from production to storage, transport, and final distribution. Hydrogen blended into natural gas introduces additional challenges, since existing pipeline infrastructure was not originally designed for hydrogen, making rigorous analytical control essential for preventing corrosion, equipment malfunction, and safety issues.</p><p>To address these challenges, Agilent presents a comprehensive suite of GC-based hydrogen testing workflows. The compendium showcases key analytical instruments—such as the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=8890"><strong>Agilent 8890 GC</strong></a>, <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=8355+SCD"><strong>8355 SCD</strong></a>, 8255 NCD, <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=5977C"><strong>5977C GC/MSD</strong></a>, and portable <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=990+Micro+GC"><strong>990 Micro GC</strong></a>—each tailored for detecting critical impurities at trace levels in accordance with ISO 14687-2019, SAE J2719, and other global standards. Featured application notes demonstrate capabilities including ultratrace ammonia monitoring, analysis of sulfides and halides, sulfur speciation, and fast impurity screening for hydrogen and natural gas streams.</p><p>Beyond instrumentation, the brochure outlines Agilent’s service ecosystem supporting method deployment, instrument verification, sustainability strategies, and lab operations management through CrossLab services and OpenLab software. These include preventive maintenance programs, financial solutions, certified pre-owned instruments, and consulting for analytical method development.</p><p>Finally, the brochure connects hydrogen-fuel purity testing with broader sustainability goals. Agilent encourages laboratories to adopt circular-economy practices—reducing waste, extending instrument lifecycles, and improving energy efficiency—emphasizing that clean hydrogen starts with responsible, efficient, and reliable laboratory workflows.</p><h3><strong>2. LECO / MDCW: BOOSTING NON-TARGETED ANALYSIS WITH COMPREHENSIVE TWO-DIMENSIONAL GAS CHROMATOGRAPHY AND HIGH-RESOLUTION MASS SPECTROMETRY</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/FL_18_Sebastiano_b4cf417f82.pdf"><strong>Full PDF for download</strong></a></li></ul><p>The presentation by <strong>Sebastiano Panto (LECO EATC Berlin)</strong> focuses on demonstrating how <strong>comprehensive two-dimensional gas chromatography coupled with high-resolution time-of-flight mass spectrometry (</strong><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?instrumentationItems=2-13-3&amp;mainauthorItems=24"><strong>GC×GC-HR-TOFMS</strong></a><strong>)</strong> significantly enhances non-targeted and targeted screening workflows, particularly in environmental analysis. Using liver extracts from <strong>Glaucous gulls (Larus hyperboreus)</strong> from the Svalbard region as a case study, the work aims to reveal contamination patterns and improve compound identification confidence.</p><p>Sample preparation included homogenization, lipid removal, and multi-step cleanup involving <strong>GPC/SEC chromatography</strong> and Florisil fractionation, yielding separate non-polar and polar fractions for analysis (page 4). Analytical separations were performed on an <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=8890+GC"><strong>Agilent 8890 GC</strong></a> equipped with a dual-column GC×GC setup (Rxi-5SilMS and Rxi-17SilMS), cryogenic modulation, and Helium carrier gas. Detection used the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=24&amp;search=Pegasus+HRT%2B4D+HR-TOFMS"><strong>LECO Pegasus® HRT+4D HR-TOFMS</strong></a> with multiple ionization modes—<strong>EI, PCI, and ECNI</strong>—enabling simultaneous acquisition of structural, isotopic, and exact-mass information (page 5).</p><p>The results highlight the advantages of GC×GC-HR-TOFMS in non-target screening: improved separation patterns, higher library match scores, exact-mass confirmation, and enhanced structural elucidation. Electron ionization (EI) provided clean spectra with high match scores for classic pollutants (e.g., PCBs, DDE), while <strong>electron capture negative ionization (ECNI)</strong> greatly improved selectivity and sensitivity for halogenated contaminants such as toxaphenes and brominated flame retardants, enabling confident identification even when EI spectra were ambiguous (pages 6–13). The instrument’s high mass accuracy and isotopic fidelity are shown to be essential for distinguishing closely related halogenated compounds.</p><p>The study concludes that combining <strong>GC×GC separation power</strong> with <strong>HR-TOFMS accurate-mass detection</strong> and complementary ionization modes offers a robust discovery platform for environmental exposomics. This analytical workflow supports more confident annotation of persistent organic pollutants (POPs) and emerging contaminants in complex biological matrices, ultimately helping assess ecological risks in sensitive Arctic ecosystems where these avian species reside (page 15).</p><h3><strong>3. Shimadzu: High-Sensitivity Gas Analysis Using the GCMS-QP2050 and GI-30 Auto Gas Injector</strong></h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_01_00953_en_7e1a865aae.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Gas analysis is conducted across a wide range of fields, including resources, energy, and the environment. Typical targets include inorganic gases such as H2, CO, and CO2, and light hydrocarbon gases starting with CH4, with analyses primarily performed using GC. In Application News No. 01- 00858, examples of gas sample analysis using TCD and BID installed on the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=1&amp;search=Brevis+GC-2050"><strong>Brevis GC-2050</strong></a> were presented.&nbsp;</p><p>However, qualitative analysis by GC requires standard substances, making the identification of unknown impurities in gas samples difficult. Furthermore, in inorganic gas analysis, complete chromatographic separation of peaks can be challenging, and when GC fails to fully separate them, both qualitative and quantitative analysis become difficult.&nbsp;</p><p>In contrast, gas analysis using GC-MS enables qualitative identification of unknown components without standard substances through mass spectral library searches. Quantitation in GC-MS is performed using mass chromatograms, allowing accurate measurements even when peaks overlap.&nbsp;</p><p>In this Application News, high-sensitivity analysis of inorganic gases and light hydrocarbon gases was performed using the compact yet high-performance <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=1&amp;search=GCMS-QP2050"><strong>GCMS-QP2050</strong></a>. Gas samples were introduced using the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=1&amp;search=GI-30"><strong>GI-30 Auto Gas Injector</strong></a>, enabling automated, continuous analysis and delivering higher reproducibility than manual sample injection.</p><h4><strong>Instrument Configuration and Analytical Conditions&nbsp;</strong></h4><p>A 10 ppm standard mixed gas sample in a cylinder was analyzed using the GCMS-QP2050. Gas sample injection into the GC-MS was performed with the GI-30 Auto Gas Injector (P/N: S221- 89755-41). The instrument configuration is shown in Fig. 1. The analytical conditions used are summarized in Table 1. Under typical ionization settings (ionization voltage 70 V and emission current 60 µA), ionization of the helium carrier gas generates a significant signal at m/z 2, making detection of H2 (monitor ion: m/z 2) difficult. Therefore, for analysis in SIM mode, the ionization voltage was set to 20 V and the emission current to 20 µA to suppress He ionization.</p><h4><strong>Automated Continuous Analysis Using the GI-30&nbsp;</strong></h4><p>The GI-30 Auto Gas Injector is a sample pretreatment device that automatically introduces a fixed volume of gas into the GC. It is used by connecting either a gas cylinder or a sample bag. When the GI-30 is connected to a gas cylinder, automated, continuous analysis of gassamples becomes possible.&nbsp;</p><p>The GI-30 is equipped with an optional valve purge mechanism. Purging the internal valve with gas reduces the ingress of ambient air. This is effective for analyzing components in ambient air, such as N2 and O2, as well as for measuring tracelevel components.&nbsp;</p><p>Table 2 shows the peak-area repeatability (%RSD) obtained when a 10 ppm standard mixed gas was analyzed automatically and continuously in SIM mode. As an example, an overlay of the CH4 SIM chromatograms is shown in Fig. 3. Because the GI-30 meters a fixed volume of gas into the GC via a sample loop, excellent reproducibility was achieved for all compounds.</p><h4><strong>Conclusion&nbsp;</strong></h4><p>Using the GCMS-QP2050, high-sensitivity analysis of inorganic gases, such as H2, and light hydrocarbons was achieved. Gas sample injection was performed with the GI-30 Auto Gas Injector, enabling automated, continuous analysis and delivering higher reproducibility compared with manual sample injection. The compact, high-performance GCMS-QP2050, together with the GI-30, enables automation and high-precision gas analysis, and supports greater efficiency in GC-MS-based gas analysis.</p><h3><strong>4. Thermo Fisher Scientific: Trace analysis of epichlorohydrin in drinking water using GC-MS coupled with purge and trap</strong></h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_003894_gc_single_quad_isq_7610_environmental_an003894_na_en_70123385ae.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Epichlorohydrin (ECH) is a versatile starting material in the production of drugs and polymers and is also used as an insect fumigant and solvent for organic synthesis reactions. ECH-based polymer pipes are commonly used in the production of drinking water due to their durability and resistance to corrosion. However, ECH is known for its high reactivity and toxicity, which poses significant health risks if it contaminates drinking water. Exposure to ECH can cause respiratory issues, skin irritation, and has been classified as a probable human carcinogen.</p><p>Due to these risks, many countries have imposed strict limits on the amount of ECH allowed in drinking water. Recently, Europe set a minimum detection limit (MDL) of 30 parts per trillion (ppt) for ECH in drinking water.2 Whereas typically required detection limits for most compounds mandated for analysis in Europe can be achieved using methods based on static headspace, the stringent MDL required for ECH requires preconcentration, for example using purge and trap (P&amp;T) technology.3,4 This technology involves purging the water sample with an inert gas to release volatile organic compounds (VOCs), which are then trapped and concentrated for analysis, ensuring reliable detection at very low concentrations. In the United States, the analysis of VOCs in drinking water is mandated by the Environmental Protection Agency (EPA). The EPA requires the use of P&amp;T technology for drinking water analysis to ensure that even trace amounts of harmful compounds like ECH are detected and managed appropriately.&nbsp;</p><p>The following evaluation describes the use of the ISQ 7610 Single Quadrupole MS system coupled with the Thermo Scientific™ TRACE™ 1610 GC with the Thermo Scientific™ HeSaver-H2 Safer™ split/splitless injector and Teledyne LABS Tekmar Lumin P&amp;T concentrator combined with the AQUATek LVA autosampler for the analysis of ECH in drinking water.</p><h4><strong>Experimental</strong></h4><h5><strong>GC-MS parameters&nbsp;</strong></h5><p>A <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/486"><strong>TRACE 1610 GC</strong></a> was coupled to the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/484"><strong>ISQ 7610 MS</strong></a> equipped with the Thermo Scientific™ NeverVent ™ vacuum probe interlock (VPI) and an ExtractaBrite ion source. A <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/1773"><strong>Thermo Scientific™ TraceGOLD™ TG-VMS column</strong></a>, 30 m × 0.25 mm, 1.4 µm film (P/N 26080-3320) was used for compound separation. The HeSaver-H2 Safer SSL injector was utilized to reduce the carrier gas consumption by decoupling the gas used for the chromatographic separation from the gas used to pressurize the inlet and maintain split and purge flows. The critical separations were maintained with a run time of under 15 minutes.</p><p>For this analysis, the ISQ 7610 MS was operated in Selected Ion Monitoring (SIM) mode for increased selectivity, as required for this application. Extended method parameters for the ISQ 7610 MS are shown in Table 2.</p><h5><strong>Instrument control and data processing&nbsp;</strong></h5><p>Data was acquired, processed, and reported using the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/76"><strong>Thermo Scientific™ Chromeleon™ Chromatography Data System (CDS)</strong></a>. This software can control both the GC-MS system and the Tekmar Lumin P&amp;T with the AQUATek LVA. This allows a single software to be utilized for the full workflow, simplifying the instrument operation. This application note is available for download via the Thermo Scientific™ AppsLab Library, which contains all the parameters needed to acquire, process, and report the analytical data for analysis of ECH.5</p><h4><strong>Conclusion&nbsp;</strong></h4><p>This study demonstrates the capability of the Tekmar Lumin P&amp;T with the AQUATek LVA system connected to the ISQ 7610 Single Quadrupole GC-MS to detect and quantify low-level ECH in drinking water samples, in compliance with EPA requirements.&nbsp;</p><ul><li>Utilizing the Tekmar Lumin P&amp;T’s ability to purge with nitrogen, along with using the HeSaver-H₂Safer SSL injector, nearly four times less helium was consumed during the analysis without sacrificing system performance.&nbsp;</li><li>The linearity of the calibration curve from 30 ppt to 5,000 ppt passed method requirements.</li><li>The application proved robust during an extended study with 20 samples of a 1,000 ppt ECH standard injected over a series of 124 injections, obtaining 4.4% precision and 118% accuracy of the recovery.</li></ul>

News from LabRulezGCMS Library - Week 48, 2025

<p><strong>In the week of December 1, the following webinars await you in the field of gas / solid phase and especially Raman, FTIR, GC and GC/MS.</strong></p><blockquote><h4><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/webinars"><strong>👉 DETAILS AND REGISTRATION IN THE WEBINARS SECTION</strong></a></h4><p><strong>👉 Search and filter in the largest global database</strong> with over <strong>5 000 GC, LC, MS and spectroscopy webinars</strong>.</p></blockquote><div><div><div><div><div><div><h5><strong>1. Wasson-ECE Instrumentation: Sample Capture, Transport and Introduction</strong></h5><ul><li>Tu, 2.12.2025 21:30 CET</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/webinar/5528">Registration</a></li></ul><p>Explore best practices for sample capture, transport, and introduction to ensure accuracy, integrity, and reliability in analytical workflows and laboratory applications.</p><h5><strong>2. Agilent Technologies: Plastic Circularity – Pyrolysis and Workflow Solutions</strong></h5><ul><li>We, 3.12.2025 07:30 CET</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/webinar/5544">Registration</a></li></ul><p>Learn how Agilent GC solutions support plastic waste pyrolysis by characterizing oils, quantifying hydrocarbons, and detecting contaminants for reuse.</p><h5><strong>3. C&amp;EN: Inline Raman – Avoid the Million-Dollar Product Mix-Up</strong></h5><ul><li>We, 3.12.2025 19:00 CET</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/webinar/5700">Registration</a></li></ul><p>Learn how inline Raman spectroscopy eliminates costly product mix-ups by enabling rapid, on-stream material identification. Experts from HF Sinclair and Metrohm USA share real-world strategies and ROI insights.</p><h5><strong>4. Thermo Fisher Scientific: Every Wafer Counts – How ppt-Level Gas Analysis Safeguards Semiconductor Production</strong></h5><ul><li>Th, 4.12.2025 16:00 CET</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/webinar/5702">Registration</a></li></ul><p>Safeguarding semiconductor production demands ppt-level gas purity. Learn how APIX δQ and Quattro mass spectrometers deliver ultra-fast, ultra-sensitive UHP gas analysis to protect every wafer.</p><h5><strong>5. AZoM: Polymer Upcycling via Reactive Extrusion – FTIR Microscopy Insights into Blend Compatibilization</strong></h5><ul><li>Th, 4.12.2025 17:00 CET</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/webinar/5652">Registration</a></li></ul><p>Discover how reactive extrusion and FTIR microscopy enable sustainable upcycling of reprocessed polypropylene. Learn to optimize extrusion parameters and enhance polymer blend performance.</p></div></div></div></div></div></div>

Webinars LabRulezGCMS Week 49/2025

<p><strong>Natural rose extracts are highly valued yet prone to adulteration, making robust analytical tools essential for verifying authenticity. In this study, GC-MS was used to characterize rose fragrances and quantify major rose alcohols, including phenyl ethyl alcohol, citronellol, and geraniol. Standard accords composed of six synthetic fragrance compounds were baseline-resolved on a nonpolar column, with calibration curves established at concentrations representative of commercial samples. Principal component analysis (PCA) further differentiated accords based on their chemical signatures.</strong></p><p>To capture the volatile bouquet, HS-SPME was applied to fragrance strips and commercial materials, including rose absolute, rose oil, a perfume, and a peony flower. Both liquid injection and HS-SPME approaches provided complementary qualitative and quantitative insights. Overall, the results demonstrate the applicability of GC-MS and HS-SPME for evaluating rose alcohol composition in complex fragrance matrices and for identifying potential adulteration.</p><blockquote><h4><strong>The original article</strong></h4><h4><a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/10.1021/acsmeasuresciau.5c00112"><strong>Determination of Rose Alcohol Composition in Extracts and Flowers via Headspace Solid-Phase Microextraction and GC-MS</strong></a></h4><p>Amber M. Hupp*</p><p>ACS Meas. Sci. Au 2025</p><p><a target="_blank" rel="noopener noreferrer" href="https://doi.org/10.1021/acsmeasuresciau.5c00112">https://doi.org/10.1021/acsmeasuresciau.5c00112</a></p><h6>licensed under <a target="_blank" rel="noopener noreferrer" href="https://creativecommons.org/licenses/by/4.0/"><strong>CC-BY 4.0</strong></a></h6></blockquote><p><strong>Selected sections from the article follow. Formats and hyperlinks were adapted from the original.</strong></p><p>With the availability of routine synthetic methods, some fragrance houses will opt to utilize entirely synthetic accords that replicate the desired olfactory profile of rose. These accords typically include synthetic versions of the three rose alcohols in varying proportions, along with other compounds found in natural rose (e.g., eugenol, linalool, rose oxide) or those that contribute specific aromatic facets (e.g., dimethyl acetaldehyde phenyl acetate (PADMA) or cis-3-hexenal for a green note). Such accords may also incorporate natural oils or isolated molecules (isolates) from natural oils. Many of these components have been studied for their olfactory contributions to rose accords. <a href="javascript:void(0);">(10)</a></p><p>The most commonly employed instrumental technique for determining the composition of volatile fragrance compounds is gas chromatography, typically coupled with Mass Spectrometry (GC-MS). In this technique, fragrance oils and absolutes are diluted in an organic solvent and analyzed for both qualitative identification of chemical composition and quantitative determination of concentration. GC-MS is widely used in the literature for analyzing rose oils and absolutes, and although proprietary methods are rarely published, GC-MS remains the preferred instrumental technique in major fragrance houses. <a href="javascript:void(0);">(4,5,8,10,11)</a></p><p>As with all volatile mixtures, the headspace vapor above a liquid exhibits a different component ratio than the liquid itself, in accordance with Raoult’s Law. Variations in the vapor pressure cause certain components to be either enriched or diminished in the vapor phase. This phenomenon has prompted interest in analyzing the headspace of fragrance materials. A widely adopted method for such analysis is solid-phase microextraction (HS-SPME). <a href="javascript:void(0);">(12)</a> In this approach, a specialized fiber is exposed to the vapor phase above a liquid or solid sample, where volatile compounds adsorb onto the fiber’s surface. The fiber is then inserted into the GC-MS injection port, where the volatiles are thermally desorbed and introduced into the chromatographic column. HS-SPME has proven effective for profiling the aroma of rose alcohols in flowers and other fragrant materials. <a href="javascript:void(0);">(13−15)</a> Moreover, HS-SPME is valuable for analyzing solid samples that are otherwise difficult to assess via conventional GC-MS. Examples include fresh roses on the bush, freshly cut flowers, and commercial products such as lotions and candles. <a href="javascript:void(0);">(3,9)</a> Most published HS-SPME studies examined samples in isolation, either the oil or the headspace, the flower or the oil, or the oil versus the absolute, rather than analyzing both simultaneously. Consequently, methodologies vary across research groups. Furthermore, no published data currently address how the composition of rose alcohols may differ from the liquid oil or absolute to its corresponding headspace of the oil or absolute or between the flower and the resulting extract.</p><p>This study presents a method for analyzing both liquid and headspace rose samples applicable throughout the production process of commercial rose materials. The objectives of this experiment are (1) to develop a method for quantifying rose alcohols in liquid products (naturals and synthetics); (2) to establish a technique for identifying volatile components via headspace sampling of liquids (oils, absolutes, perfumes) and solid materials (scent strips, flowers); and (3) to investigate the influence of extraction time on the analysis of rose alcohols in the vapor phase. A unified method applicable across all material types, from the rose flower to the natural oil product to the final fragrance product represents a significant advancement in detecting adulteration and assessing rose alcohol content in situ and has not been previously documented.</p><h3><strong>Materials and Methods</strong></h3><h4><strong>Instrumentation</strong></h4><p>Separations were performed by using an <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=6890"><strong>Agilent 6890 gas chromatograph</strong></a> coupled with an <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=5973"><strong>Agilent 5973 mass spectrometer</strong></a> (Agilent Technologies, Santa Clara, TX). The GC was equipped with a nonpolar ZB-5 column (5% phenyl polydimethylsiloxane, Phenomenex, 30 m × 0.25 mm × 0.25 μm i.d.). The oven temperature was optimized for separation of the six components in the rose accord as follows: 100 to 200 °C at 10 °C/min, yielding a total run time of 10.0 min. High purity helium was used as a carrier gas at a flow rate of 0.8 L/min. Each liquid sample was manually injected (1 μL from 10 μL syringe, Hamilton Company) with a split ratio of 200:1. Each headspace sample was desorbed from the SPME fiber by using a split ratio of 50:1. The inlet and transfer line temperatures were held at 250 and 280 °C, respectively. An electron-impact ionization source was utilized with a quadrupole mass analyzer operated in full-scan mode (<i>m</i>/<i>z</i> 40 – 600) with a sampling rate of 2.6 scans/s. The mass spectrometer source and quadrupole were held at 230 and 150 °C, respectively.</p><p>Peak identification was performed using a NIST database (NIST14, Gaithersburg, MD) as well as retention time and mass spectral comparisons to external standards. The area of each peak was identified via integration using a common threshold (Enhanced Chemstation D.03.00.611, Agilent). For chemometric analysis, peak areas were normalized using the total area under the chromatogram in Microsoft Excel 2016. Normalized peak areas were mean-centered in Pirouette 4.5 (Infometrix, Bothell, WA) prior to subsequent chemometric analysis. All figures were created using the plotting feature in Microsoft Excel.</p><h4><strong>Part 2. SPME Headspace Analysis</strong></h4><p>Sampling the headspace above a natural extract or perfume is advantageous, as only the volatile components in the sample are analyzed and materials can be sampled in situ. Using SPME, the headspace above each standard and commercial sample was analyzed for percent composition and compared to direct liquid injection results. A time-based extraction study was conducted, with two time points illustrated in <a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/10.1021/acsmeasuresciau.5c00112#fig5">Figure 5</a> and <a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/10.1021/acsmeasuresciau.5c00112#tbl4">Table 4</a>. Within 20 min, the more volatile PEA and citronellol were readily extracted by the SPME fiber, while the least volatile components produced only small peaks. Over time, the remaining six components become more prominent. By the 2 h mark, the peak ratios more closely resembled those observed in the liquid samples (see <a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/10.1021/acsmeasuresciau.5c00112#fig1">Figure 1</a>). This shift indicates that the ratio of PEA to the other components changes over time, as equilibrium is not yet established at the 20 min time point.</p><p><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/ACS_Meas_Sci_Au_2025_Figure_5_Chromatography_of_standard_rose_A_using_SPME_for_20_min_and_2_h_107eebedb5.jpg" alt="ACS Meas. Sci. Au 2025: Figure 5. Chromatography of standard rose A using SPME for 20 min and 2 h." srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_ACS_Meas_Sci_Au_2025_Figure_5_Chromatography_of_standard_rose_A_using_SPME_for_20_min_and_2_h_107eebedb5.jpg 222w," sizes="100vw" width="1500" height="1055"></p><p>Several factors contribute to the low extraction efficiency of the least volatile components. First, differences in volatility play a key role. Larger molecules with lower vapor pressures require more time to enter the vapor phase. Second, in this study, the least volatile components were also present at low concentrations. According to Raoult’s law, components with both low concentration and low vapor pressure will be underrepresented in the headspace relative to the liquid. Third, only one type of SPME fiber was used; alternative fiber chemistries may be better suited for capturing the lower volatility compounds. Lastly, the samples were neither agitated nor heated during extraction, both known factors to accelerate equilibrium. To improve extraction of less volatile components, it is hypothesized that extended extraction time, agitation, or heating would be beneficial, assuming concentration and fiber chemistry remain constant. However, the objective of this study was not to reach equilibrium, but rather to assess whether the percent composition of rose alcohols could be determined using a rapid extraction method comparable in duration to direct liquid injection. Since rose alcohols are the most volatile of the six components in the standard, a shorter extraction time point was appropriate for this analysis.</p><p>Headspace analysis of the commercial samples was conducted using the same 20 min SPME extraction method. Chromatograms for the rose absolute and rose oil are presented in <a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/10.1021/acsmeasuresciau.5c00112#fig7">Figure 7</a>, while for the chromatogram for the rose perfume is shown in <a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/10.1021/acsmeasuresciau.5c00112#fig8">Figure 8</a>. As observed previously, the rose absolute consists predominately of the three rose alcohols, whereas the rose oil contains a broader array of volatile constituents. Peak intensities and areas obtained via headspace SPME differ from those observed in liquid injection, with early eluting components exhibiting enhanced signals and later eluting components being underrepresented. Nonetheless, the detection of later eluting peaks demonstrates potential for qualitative analysis of less volatile analytes, even under short nonequilibrium extraction conditions. The rose perfume sample yielded a complex chromatographic profile with numerous peaks and relatively low concentrations of the three rose alcohols, consistent with results from liquid-phase analysis. Notably, the application of HS-SPME to a fragrance strip sprayed with perfume represents a novel analytical approach, as it has not been documented in existing literature.</p><p><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/ACS_Meas_Sci_Au_2025_Figure_7_Chromatograms_of_headspace_analysis_by_SPME_of_rose_absolute_and_rose_oil_16013a9dbb.jpg" alt="ACS Meas. Sci. Au 2025: Figure 7. Chromatograms of headspace analysis by SPME of rose absolute and rose oil." srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_ACS_Meas_Sci_Au_2025_Figure_7_Chromatograms_of_headspace_analysis_by_SPME_of_rose_absolute_and_rose_oil_16013a9dbb.jpg 218w," sizes="100vw" width="1500" height="1073"></p><p><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/ACS_Meas_Sci_Au_2025_Figure_8_Chromatogram_of_headspace_analysis_by_SPME_of_peony_flower_db0b14322a.jpg" alt="ACS Meas. Sci. Au 2025: Figure 8. Chromatogram of headspace analysis by SPME of peony flower and rose parfum. The rose alcohols are identified as 1-PEA, 2-citronellol, and 3-geraniol." srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_ACS_Meas_Sci_Au_2025_Figure_8_Chromatogram_of_headspace_analysis_by_SPME_of_peony_flower_db0b14322a.jpg 234w," sizes="100vw" width="1488" height="992"></p><h3><strong>Conclusions</strong></h3><div><p>This study presents a robust analytical method for the quantitation of three rose alcohols, phenyl ethyl alcohol, citronellol, and geraniol, in natural rose extracts, commercial perfumes, and botanical samples. Liquid injection provided the most accurate representation of the original liquid formulations, serving as a benchmark for comparison. PCA effectively clustered rose accord standards based on the percent composition of rose alcohols and minor chemical constituents, demonstrating its utility in distinguishing sample categories and chemical profiles.</p><p>Calibration of the percent area for each rose alcohol was successfully achieved across both natural and synthetic materials without the use of an internal standard. In cases where direct liquid sampling is impractical or the sample is nonliquid, headspace analysis via HS-SPME offers a viable alternative. HS-SPME enabled rapid and effective detection of the target rose alcohols in various commercial products along with additional volatile components. While calibration accuracy decreased with increasing sample complexity, particularly in matrices containing numerous volatile compounds, the method remained capable of estimating rose alcohol percentages and identifying supplementary peaks. Notably, headspace analysis of a fresh peony flower confirmed the presence of all three rose alcohols, underscoring the potential of HS-SPME for analyzing solid botanical samples. Overall, this approach enables the determination of rose alcohol concentrations in both liquid and headspace of diverse sample types. The method offers a promising tool for monitoring compositional changes throughout the production process of rose-derived materials and may aid in the detection of adulteration in essential oils and absolutes.</p></div>

Determination of Rose Alcohol Composition in Extracts and Flowers via Headspace Solid-Phase Microextraction and GC-MS

<p><strong>Our Library never stops expanding. What are the most recent contributions to LabRulezGCMS Library in the week of 1st December 2025? Check out new documents from the field of the gas phase, especially GC and GC/MS techniques!</strong></p><blockquote><p><span style="font-size:20px;">👉 </span><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library"><span style="font-size:20px;"><strong>SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT GCMS AND RELATED TECHNIQUES</strong></span></a></p></blockquote><blockquote><p><strong>👉 Need info about different analytical techniques?</strong> Peek into <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library"><strong>LabRulezLCMS</strong></a> or <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library"><strong>LabRulezICPMS</strong></a> libraries.</p></blockquote><p>This week we bring you application notes by <strong>Agilent Technologies, Shimadzu </strong>and<strong> Thermo Fisher Scientific </strong>and presentation by<strong> LECO /MDCW!</strong></p><h3><strong>1. Agilent Technologies: Analysis of 197 Pesticides in Durian by Agilent PAL 3 Autosampler and 7000E Triple Quadrupole GC/MSD</strong></h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_197_pesticides_durian_pal3_7000e_gc_msd_5994_8702en_agilent_e5a68eaf99.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Pesticide residue analysis in food products is critical to ensuring consumer safety and regulatory compliance. Durian (Durio zibethinus), known as the "king of fruits" and widely exported across Southeast Asia, China, and beyond, presents unique analytical challenges due to its sulfur-rich compounds, high fat content, and complex volatile matrix. Comprehensive pesticide analysis in such matrices demands highly sensitive, selective, and robust analytical solutions. The European Union Reference Laboratories (EURL) SANTE/11312/2021 guidelines set rigorous performance criteria for pesticide residue analysis, including strict requirements for method accuracy, precision, and sensitivity.1 Laboratories need to achieve recoveries between 70% to 120%, precision (RSD) below 20%, and quantification limits at or below regulatory maximum residue limits (MRLs), even in complex food matrices such as durian. This application note demonstrates a high-performance workflow for the analysis of 197 pesticides in durian using an Agilent PAL3 Autosampler combined with an Agilent 7000E Triple Quadrupole GC/MSD system. The PAL3 Autosampler provides high-throughput, precise sample handling, while the 7000E GC/MSD offers exceptional sensitivity and reproducibility for trace-level pesticide quantification. Optimized sample preparation and instrumental conditions ensure reliable performance, meeting and exceeding SANTE criteria for method validation.</p><h4><strong>Experimental</strong></h4><h5><strong>PAL 3 RTC and 7000E GC/TQ parameters&nbsp;</strong></h5><p>The analysis parameters are shown in Table 1. The target and ISTD compound MRM parameters are listed in Appendix&nbsp;1. Figure 1 shows a typical MRM chromatogram of targeted pesticides spiked in durian at a concentration of 100 ppb.</p><ul><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=PAL+3"><strong>Agilent PAL 3 (Liquid Tool)</strong></a></li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=8890"><strong>Agilent 8890 GC</strong></a></li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=7000E"><strong>Agilent 7000E</strong></a></li></ul><h4><strong>Conclusion&nbsp;</strong></h4><p>This study successfully demonstrated a robust and sensitive method for the quantitative analysis of 197&nbsp;pesticides in durian using an Agilent PAL3 Autosampler combined with an Agilent&nbsp;7000E Triple Quadrupole GC/MSD system. The optimized workflow, including sample extraction with an Agilent Bond Elut QuEChERS EN kit followed by cleanup with the Highly Pigmented dSPE kit, provided excellent recovery and precision. All target pesticides showed analysis accuracy between 80% and 120% and RSD values below 10% at a spiked level of 10 ppb. The results confirm the method's suitability for routine high-throughput pesticide quantification in complex matrices such as durian. The use of matrix-matched calibration and matrix‑optimized MRMs further ensured accurate and reproducible quantitation, reinforcing the method's applicability for regulatory and food safety testing.</p><h3><strong>2. LECO / MDCW: Applying statistical data processing tools for GC×GC differentiation of alternative aviation fuels</strong></h3><ul><li>Presentation</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/FL_18_Sebastiano_b4cf417f82.pdf"><strong>Full PDF for download</strong></a></li></ul><p>The presentation introduces LECO’s long-standing role in separation science and its evolution from elemental analyzers to advanced mass spectrometry platforms. A key emphasis is placed on LECO’s innovations in <strong>time-of-flight mass spectrometry (TOFMS)</strong>, including the Pegasus series and the new <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=24&amp;search=Pegasus+BTX"><strong>Pegasus BTX</strong></a>, a benchtop TOFMS offering high sensitivity, rugged detector technology, fast spectral acquisition (1–500 spectra/s), and broad mass range (10–1500 m/z). This technological foundation supports comprehensive <strong>GC×GC-MS</strong> workflows essential for analyzing chemically complex matrices such as aviation fuels.</p><p>A major focus of the talk is on <strong>software tools</strong> for non-targeted data processing. LECO’s software ecosystem—<a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=24&amp;search=ChromaTOF"><strong>ChromaTOF</strong></a><strong>, ChromaTOF Tile, and </strong><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=24&amp;search=ChromaTOF+Sync"><strong>ChromaTOF Sync</strong></a>—enables detailed deconvolution, quantitation, high-resolution spectral analysis, and especially <strong>statistical comparison of GC×GC datasets</strong>. ChromaTOF Tile uses a chromatographic “tiling” strategy to link datasets and detect differences between sample groups using three statistical metrics: <strong>Fisher Ratio</strong>, <strong>Coefficient of Variation (CoV)</strong>, and <strong>Fold-Change</strong>. Each metric serves a different experimental purpose, from comparing traditional vs. synthetic jet fuels (Fisher Ratio) to exploring variability among multiple alternative fuel processes (CoV), or identifying additive components in two-sample comparisons (Fold-Change).</p><p>The presentation demonstrates how raw GC×GC-MS data are curated into <strong>feature tables</strong>, statistically evaluated, and visualized in <strong>PCA plots, bar charts, and chromatographic overlays</strong>. For example, Fisher Ratio comparison highlights statistically significant chemical differences between conventional Jet A and synthetic fuels, while CoV analysis reveals clustering patterns among diverse synthetic fuel production pathways such as <strong>LT-FT SPK, HT-FT SPK, HEFA, SIP, ATJ, and CHJ</strong>. These workflows enable analysts to rapidly identify biomarkers or distinguishing compositional features within highly complex hydrocarbon matrices.</p><p>Ultimately, the talk demonstrates that choosing the correct statistical processing method can dramatically simplify interpretation of complex GC×GC-MS datasets. LECO’s integrated instrumentation—particularly the Pegasus BTX TOFMS—and software platforms together provide a powerful toolkit for fuel characterization, quality evaluation, and differentiation of emerging <strong>alternative aviation fuels</strong>. By combining comprehensive chromatography with robust statistical approaches, researchers can gain deeper insights into chemical variability, production signatures, and additive packages in modern aviation fuel technologies.</p><h3><strong>3. Shimadzu: Analysis of Formic Acid in Acetone Using GC/MS System</strong></h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_01_00957_en_e8b083b86e.pdf"><strong>Full PDF for download</strong></a></li></ul><p>In research on artificial photosynthesis, the analysis of impurities in chemical products and raw materials has increased the demand for high-sensitivity analysis of formic acid. Previous examples of formic acid analysis using GC-BID and GC-FID (Jetanizer ) have been presented, but in this article high-sensitivity analysis of formic acid using the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=1&amp;search=GCMS-QP2050"><strong>GCMS-QP2050</strong></a> (see Fig. 1) isintroduced.</p><h4><strong>Insert, Column Phosphoric Acid Treatment&nbsp;</strong></h4><p>Formic acid is known to adsorb onto the injection port and column, making peak detection difficult. However, by performing phosphoric acid treatment on the glass insert and column before measurement, good peaks can be obtained. The procedure for phosphoric acid treatment of the glass insert is shown in Fig. 2, and the procedure for phosphoric acid treatment of the column isshown in Fig. 3.</p><h4><strong>Conclusion&nbsp;</strong></h4><p>By performing phosphoric acid treatment on the insert and column, it became possible to analyze formic acid in SIM mode down to 0.2 ppm. Furthermore, good results could be obtained for both linearity and repeatability. Additionally, by analyzing in Scan mode, identification of unknown peaks other than formic acid was also achieved.</p><h3><strong>4. Thermo Fisher Scientific: Uninterrupted analysis of VOCs according to U.S. EPA Method 8260C using purge and trap and single quadrupole GC-MS technology</strong></h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_001018_gc_voc_analysis_gc_ms_epa_8260c_an001018_na_en_269857401c/an-001018-gc-voc-analysis-gc-ms-epa-8260c-an001018-na-en.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Volatile organic compounds, or VOCs, are human-made contaminants used and produced in the processing of, or as, paints, adhesives, petroleum products, pharmaceuticals, and refrigerants. Many of these compounds contaminate our environment and may cause negative health effects in humans and other living beings. Analytical laboratories must monitor a variety of sample types from the environment to ensure the public are not exposed to elevated levels of VOCs. The latest version of applicable method in the United States, U.S. EPA Method 8260C, is applicable when monitoring a variety of solid waste matrices for the presence of VOCs.</p><p>To perform U.S. EPA Method 8260C, all method acceptance criteria must be achieved. These criteria include calculating the mean response factor and the relative standard deviation (RSD) of the response factors for target analytes. The RSD should be &lt;20%, with minimum response factors (RF) and MDLs for a wide range of target compounds. The analytical method must produce consistent results and be reproducible from day to day, with a continuing calibration verification (CCV) analyzed every 12 hours while samples are run. As the method covers varying matrices, it is important that the performance criteria are met in all samples of interest. The following evaluation describes the use of the ISQ 7610 GCMS coupled to the Atomx XYZ P&amp;T for U.S. EPA Method 8260C.</p><h4><strong>Experimental</strong></h4><h5><strong>Instrument control and data processing&nbsp;</strong></h5><p>Data were acquired, processed, and reported using <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/76"><strong>Chromeleon CDS software</strong></a>, version 7.2. This software can control both the GC-MS system and the Tekmar Atomx XYZ P&amp;T. This enables a single software solution to support the full workflow, simplifying the instrument operation. The optimized method used within this application note is available for download via the Thermo Scientific™ AppsLab library. AppsLab contains all the parameters needed to acquire, process, and report the analytical data for U.S. EPA Method 8260C.2</p><h5><strong>GC-MS parameters&nbsp;</strong></h5><p>A <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/486"><strong>TRACE 1610 GC</strong></a> was coupled to the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/484"><strong>ISQ 7610 MS </strong></a>equipped with the Thermo Scientific™ NeverVent™ vacuum probe interlock (VPI) and an ExtractaBrite™ ion source. Expanded method parameters for the GC-MS system are displayed in Table 3</p><h4><strong>Conclusion&nbsp;</strong></h4><p>The combined analytical solution with the TRACE 1610 GC coupled with the ISQ 7610 system and the Atomx XYZ P&amp;T system provides clear advantages for analytical testing laboratories that analyze environmental samples following the U.S. EPA Method 8260C requirements. The modularity of the TRACE 1610 GC as well as the ISQ 7610 VPI and ExtractaBrite ion source allows users to easily service the injection ports and to exchange ionization sources and analytical columns without venting the mass spectrometer, significantly reducing instrument downtime and minimizing sample analysis interruptions. The Atomx XYZ concentrator’s efficient trap cooling design reduces sample cycle time and allows for increased sample throughput. The moisture control system improves water vapor removal thereby reducing peak interference and increasing GC column life span.&nbsp;</p><p>The experiments performed clearly demonstrate the suitability of this analytical configuration for the analysis of VOCs in various environmental samples in accordance with U.S. EPA Method 8260C with the following performance parameters as evidence:&nbsp;</p><ul><li>The ISQ 7610 VPI coupled with the Tekmar Atomx XYZ P&amp;T exceeds all the requirements outlined in U.S. EPA Method 8260C for analysis of VOCs in wastewater and solid waste.</li><li>Linearity was achieved with &lt;20%,<span>&nbsp;</span>relative standard deviation for both water and soil calibration curves for the majority of compounds.&nbsp;</li><li>The MDL and precision were assessed using n=7 replicates of a 0.2 ppb water standard and n=7 replicates of a 0.5 ppb soil standard. Calculated MDLs were &lt;0.2ppb and RSDs of calculated results were &lt;10% for most compounds in both the soil and water matrices.</li><li>System robustness was tested by continuously acquiring 240 injections of environmental samples over three days with no user intervention at all. The average %RSD of the calculated concentration was 8.30% with an average compound recovery of 90%.</li></ul>

News from LabRulezGCMS Library - Week 49, 2025

Green Ultrasound-Assisted Dispersive Liquid–Liquid Microextraction Coupled to GC–MS for Simultaneous Determination of Lipid-Peroxidation- and Maillard-Derived Carbonyl Compounds in Plant-Based Beverages

<p><strong>In the week of December 8, the following webinars await you in the field of gas / solid phase and especially Raman, FTIR, GC and GC/MS.</strong></p><blockquote><h4><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/webinars"><strong>👉 DETAILS AND REGISTRATION IN THE WEBINARS SECTION</strong></a></h4><p><strong>👉 Search and filter in the largest global database</strong> with over <strong>5 000 GC, LC, MS and spectroscopy webinars</strong>.</p></blockquote><div><div><div><div><div><div><h5><strong>1. AZoM: Achieving Net-Zero – Precision Monitoring in CCUS and Downstream Chemicals</strong></h5><ul><li>Tu, 9.12.2025 16:00 CET</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/webinar/5693">Registration</a></li></ul><p>Explore how FTIR and mass spectrometry provide real-time monitoring of CO₂ purity and impurities in CCUS pipelines, supporting safety, compliance, and efficient e-fuel production from captured carbon.</p><h5><strong>2. Wasson-ECE Instrumentation: Specialty GC Detectors – PDHID and SCD</strong></h5><ul><li>Tu, 9.12.2025 21:30 CET</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/webinar/5529">Registration</a></li></ul><p>Discover the advantages of specialty GC detectors PDHID and SCD in this webinar, covering sensitivity, selectivity, and applications in trace gas analysis.</p><h5><strong>3. Agilent Technologies: WAX Column Technology for Today’s Lab – Updates That Matter</strong></h5><ul><li>We, 10.12.2025 16:00 CET</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/webinar/5655">Registration</a></li></ul><p>Explore the latest breakthroughs in GC WAX column technology. Learn how Agilent’s DB-WAX UI, DB-FATWAX UI, and DB-HeavyWAX offer improved inertness, robustness, and low bleed for modern GC/MS workflows.</p><h5><strong>4. Agilent Technologies: Tip and Tricks – How to Best Use the Handheld Raman Vaya</strong></h5><ul><li>Th, 11.12.2025 15:00 CET</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/webinar/5747">Registration</a></li></ul><p>Join us for the second session on Vaya Method Development Tips and Tricks!</p><h5><strong>5. C&amp;EN: Unpacking Plastic Packaging – Developments in Recycled Polymer and Novel Fuel Analysis Using GC-MS</strong></h5><ul><li>Th, 11.12.2025 17:00 CET</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/webinar/5711">Registration</a></li></ul><p>Learn how GC×GC-TOF MS enhances characterization of recycled polymers and pyrolysis oils. Discover workflows that improve separation, detection, and QC to support high-quality, sustainable recycling.</p></div></div></div></div></div></div>

Webinars LabRulezGCMS Week 50/2025

<p><strong>Our Library never stops expanding. What are the most recent contributions to LabRulezGCMS Library in the week of 8th December 2025? Check out new documents from the field of the gas phase, especially GC and GC/MS techniques!</strong></p><blockquote><p><span style="font-size:20px;">👉 </span><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library"><span style="font-size:20px;"><strong>SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT GCMS AND RELATED TECHNIQUES</strong></span></a></p></blockquote><blockquote><p><strong>👉 Need info about different analytical techniques?</strong> Peek into <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library"><strong>LabRulezLCMS</strong></a> or <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library"><strong>LabRulezICPMS</strong></a> libraries.</p></blockquote><p>This week we bring you application notes by <strong>Agilent Technologies </strong>and<strong> Thermo Fisher Scientific </strong>and other document by<strong> Shimadzu!</strong></p><h3><strong>1. Agilent Technologies: High-Precision Determination of Four Greenhouse Gases in the Atmosphere Using the Agilent 8890 GC</strong></h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_monitoring_greenhouse_gas_8890_gc_5994_8744en_agilent_0e08f0909f.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Currently, China is actively implementing dual-control measures on total energy consumption and intensity. The Ministry of Ecology and Environment issued "The 14th Five-Year Plan for Ecological and Environmental Monitoring", which specifically highlights the advancement of technologies for direct measurement of carbon emissions. It calls for organizing pilot projects in multiple key industries and enterprises to monitor greenhouse gas emissions such as carbon dioxide and methane, establishing greenhouse gas monitoring networks in key cities, and upgrading the greenhouse gas monitoring capabilities of national atmospheric background stations. As a result, conducting greenhouse gas monitoring within the environmental protection stations of provinces and cities has become a critical task.</p><p>The use of GC for detecting greenhouse gases has a long history. The conventional methods used gas sampling valve for injection, TCD and FID for sequential detection of CO<sub>2</sub> and CH<sub>4</sub> , or combining a methanizer with an FID to detect CO<sub>2</sub> and CH<sub>4</sub> in one analytical channel and detecting N<sub>2</sub>O on ECD in another analytical channel.<sup>2</sup> The analytical precision for CO<sub>2</sub>, CH<sub>4</sub>, and N2 O achieved with such configurations typically ranges from 0.2% to 0.5%, but it is difficult to obtain precision better than 0.1%, which does not meet the current requirements for greenhouse gas monitoring accuracy and precision. Moreover, the traditional methods rarely report analytical precision for SF<sub>6</sub> at ppt concentration levels. To monitor trace levels of CO<sub>2</sub> , CH<sub>4</sub>, N<sub>2</sub>O, and ultratrace levels of SF<sub>6</sub> on the same GC system with high-precision results, it is necessary to optimize multiple factors included in sample injection, separation, and detection. Furthermore, the system configuration must be flexible enough to allow expansion for future analytical needs, such as incorporating trace CO analysis in air. This work demonstrates how the 8890&nbsp;GC achieves high-precision analysis of four key greenhouse gases by optimizing the injection volume, controlling injection reproducibility, and utilizing multichannel separation and high-sensitivity detectors to ensure the system runs stably in long‑term operation.</p><h4><strong>Experimental</strong></h4><h5><strong>Instrumental&nbsp;</strong></h5><p>The <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=1&amp;search=8890+GC"><strong>8890 GC</strong></a> is configured as a three-channel/multivalve/multicolumn system, enabling independent analysis of four greenhouse gases—CH<sub>4</sub> , CO<sub>2</sub> , N<sub>2</sub>O, and SF<sub>6</sub> —within 8 minutes using a single injection. The target compounds are analyzed in separate channels, reducing chromatographic peak broadening and thereby improving sensitivity and&nbsp;repeatability.&nbsp;</p><ul><li>For CO<sub>2</sub> analysis, a <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=1&amp;search=methanizer"><strong>methanizer</strong></a> is used to convert CO<sub>2</sub> to CH<sub>4</sub> , which is then detected by FID. The system eliminates the need for dehydration through backflushing and venting operation via switching valves, preventing interference from moisture and oxygen in the air and extending the lifespan of the methanizer.&nbsp;</li><li>For N<sub>2</sub>O and SF<sub>6</sub> analysis, the ECD with hidden anode design is used for high‑sensitivity detection and strong anti‑contaminant capability.&nbsp;</li><li>The CH<sub>4</sub> analysis is conducted on a single column with a dedicated large injection loop, significantly enhancing detection sensitivity and repeatability, achieving a detection limit for methane as low as single-digit ppb levels.</li></ul><h4><strong>Conclusion&nbsp;</strong></h4><p>Based on its exceptional pneumatic control and valve-based flow path design, the multivalve/multicolumn Agilent 8890 GC system achieves high-sensitivity and high-precision measurements of four key greenhouse gases. This is accomplished through optimized and precise control of sample flow rate/volume, selection of premium analytical columns, and the use of highly stable and robust FID and ECD. Standard gas samples of CO2 , CH4 , N2 O, and SF6 , with concentrations equivalent to atmospheric levels, were measured continuously 10 times. The measurement precision for these gases was better than 0.05%, 0.1%, 0.1%, and 0.5%, respectively, fully meeting the high-precision monitoring requirements of environmental monitoring stations at various levels for target greenhouse gases. Compared to other monitoring solutions, this approach is based on a stable and reliable gas chromatography platform that is technically easier to master and deploy. It represents a trusted solution developed by Agilent to assist in establishing a greenhouse gas monitoring network in China.</p><h3><strong>2. Shimadzu: GC/MS Mass Spectra Library - Polymer Additives Library Ver.2</strong></h3><ul><li>Other document</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/c146_e506_d4c93c4d60.pdf"><strong>Full PDF for download</strong></a></li></ul><h4><strong>Contains Approximately 5,800 Mass Spectra&nbsp;</strong></h4><p>This library consists of a library*, which contains 5,775 mass spectra for 590 types of polymer additives and GC/MS pyrolysates from the pyrolysis GC/MS analysis of additives, and a library containing the mass spectra for 65 compounds often targeted for analysis, selected based on their usage in the commercial market, and chemical substance regulatory information. In total, this product contains 5,840 mass spectra, which provides strong support for the analysis of polymer additives. In Ver.2, the compound registration has been newly enhanced, for example vulcanizing accelerators utilized in the rubber filed. Approximately 1,000 spectra have been added.&nbsp;</p><p><i>*ADD-MS22B F-Search Additives Library from Frontier Laboratories</i></p><h4><strong>Can Be Used with a Variety of GC/MS Systems&nbsp;</strong></h4><p>The library can be used for a variety of GC/MS applications, including pyrolysis GC/MS, which is widely used for the analysis of additives in polymer materials, and liquid sample injection GC/MS. It supports a wide range of additive analysis for customers.</p><h4><strong>Library Specifications</strong></h4><ul><li><strong>Registered compounds:</strong> 5,775+65&nbsp;</li><li><strong>Registered information:</strong> Mass spectrum, retention index for each analytical condition, compound name, molecular weight, compositional formula, structural formula, classification of additives</li><li><strong>Applicable models:</strong> <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=3&amp;search=GCMS-QP2050"><strong>GCMS-QP™ serie</strong></a>s, <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=3&amp;search=GCMS-TQ8050"><strong>GCMS-TQ™ series</strong></a> (This library does not include MS/MS spectra.)&nbsp;</li><li><strong>Pyrolyzer</strong> (Pyrolysis analysis system): <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=43&amp;search=PY-2020D"><strong>PY-2020D</strong></a>, <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=43&amp;search=PY-2020iD"><strong>PY-2020iD</strong></a>, and <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=43&amp;search=EGA%2FPY-3030D"><strong>EGA/PY-3030D</strong></a></li><li><strong>Workstations:</strong> <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=3&amp;search=GCMSsolution"><strong>GCMSsolution</strong></a>™ Ver. 4.6 and later, <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=3&amp;search=LabSolutions+GCMS"><strong>LabSolutions™ GCMS</strong></a>™ Ver. 5.131 and later, LabSolutions DB/CS GCMS Ver. 6.131 and later</li></ul><h3><strong>3. Thermo Fisher Scientific: Trace analysis of epichlorohydrin in drinking water using GC-MS coupled with purge and trap</strong></h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_003894_gc_single_quad_isq_7610_environmental_an003894_na_en_70123385ae.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Epichlorohydrin (ECH) is a versatile starting material in the production of drugs and polymers and is also used as an insect fumigant and solvent for organic synthesis reactions. ECH-based polymer pipes are commonly used in the production of drinking water due to their durability and resistance to corrosion. However, ECH is known for its high reactivity and toxicity, which poses significant health risks if it contaminates drinking water. Exposure to ECH can cause respiratory issues, skin irritation, and has been classified as a probable human carcinogen.<sup>1</sup></p><p>Due to these risks, many countries have imposed strict limits on the amount of ECH allowed in drinking water. Recently, Europe set a minimum detection limit (MDL) of 30 parts per trillion (ppt) for ECH in drinking water.<sup>2</sup> Whereas typically required detection limits for most compounds mandated for analysis in Europe can be achieved using methods based on static headspace, the stringent MDL required for ECH requires preconcentration, for example using purge and trap (P&amp;T) technology.<sup>3,4</sup> This technology involves purging the water sample with an inert gas to release volatile organic compounds (VOCs), which are then trapped and concentrated for analysis, ensuring reliable detection at very low concentrations. In the United States, the analysis of VOCs in drinking water is mandated by the Environmental Protection Agency (EPA). The EPA requires the use of P&amp;T technology for drinking water analysis to ensure that even trace amounts of harmful compounds like ECH are detected and managed appropriately.&nbsp;</p><p>The following evaluation describes the use of the ISQ 7610 Single Quadrupole MS system coupled with the Thermo Scientific™ TRACE™ 1610 GC with the Thermo Scientific™ HeSaver-H2 Safer™ split/splitless injector and Teledyne LABS Tekmar Lumin P&amp;T concentrator combined with the AQUATek LVA autosampler for the analysis of ECH in drinking water.</p><h4><strong>Experimental</strong></h4><h5><strong>GC-MS parameters&nbsp;</strong></h5><p>A <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/486"><strong>TRACE 1610 GC</strong></a> was coupled to the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/484"><strong>ISQ 7610 MS</strong></a> equipped with the Thermo Scientific™ NeverVent ™ vacuum probe interlock (VPI) and an ExtractaBrite ion source. A <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/1773"><strong>Thermo Scientific™ TraceGOLD™ TG-VMS column</strong></a>, 30 m × 0.25 mm, 1.4 µm film (P/N 26080-3320) was used for compound separation. The HeSaver-H2 Safer SSL injector was utilized to reduce the carrier gas consumption by decoupling the gas used for the chromatographic separation from the gas used to pressurize the inlet and maintain split and purge flows. The critical separations were maintained with a run time of under 15 minutes.</p><p>For this analysis, the ISQ 7610 MS was operated in Selected Ion Monitoring (SIM) mode for increased selectivity, as required for this application. Extended method parameters for the ISQ 7610 MS are shown in Table 2.</p><h5><strong>Instrument control and data processing&nbsp;</strong></h5><p>Data was acquired, processed, and reported using the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/76"><strong>Thermo Scientific™ Chromeleon™ Chromatography Data System (CDS)</strong></a>. This software can control both the GC-MS system and the Tekmar Lumin P&amp;T with the AQUATek LVA. This allows a single software to be utilized for the full workflow, simplifying the instrument operation. This application note is available for download via the Thermo Scientific™ AppsLab Library, which contains all the parameters needed to acquire, process, and report the analytical data for analysis of ECH.5</p><h4><strong>Conclusion&nbsp;</strong></h4><p>This study demonstrates the capability of the Tekmar Lumin P&amp;T with the AQUATek LVA system connected to the ISQ 7610 Single Quadrupole GC-MS to detect and quantify low-level ECH in drinking water samples, in compliance with EPA requirements.&nbsp;</p><ul><li>Utilizing the Tekmar Lumin P&amp;T’s ability to purge with nitrogen, along with using the HeSaver-H₂Safer SSL injector, nearly four times less helium was consumed during the analysis without sacrificing system performance.&nbsp;</li><li>The linearity of the calibration curve from 30 ppt to 5,000 ppt passed method requirements.</li><li>The application proved robust during an extended study with 20 samples of a 1,000 ppt ECH standard injected over a series of 124 injections, obtaining 4.4% precision and 118% accuracy of the recovery.</li></ul>

News from LabRulezGCMS Library - Week 50, 2025

<p><strong>In the week of December 15, the following webinars await you in the field of gas / solid phase and especially Raman, FTIR, GC and GC/MS.</strong></p><blockquote><h4><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/webinars"><strong>👉 DETAILS AND REGISTRATION IN THE WEBINARS SECTION</strong></a></h4><p><strong>👉 Search and filter in the largest global database</strong> with over <strong>5 000 GC, LC, MS and spectroscopy webinars</strong>.</p></blockquote><div><div><div><div><div><div><h5><strong>1. Wasson-ECE Instrumentation: O-FIDs / ASTM D5599</strong></h5><ul><li>Tu, 16.12.2025 21:30 CET</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/webinar/5530">Registration</a></li></ul><p>Learn about O-FIDs and ASTM D5599 methodology, focusing on accurate oxygenate analysis in fuels with optimized GC detector performance.</p><h5><strong>2. Agilent Technologies: Ask the Expert – Ensuring Purity and Compliance in Glycol Testing</strong></h5><ul><li>Th, 18.12.2025 10:00 CET</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/webinar/5712">Registration</a></li></ul><p>Learn how validated GC-FID workflows ensure accurate EG/DEG testing and compliance with new global regulations, including expert guidance on method setup, validation, and troubleshooting.</p><h5><strong>3. Agilent Technologies: Microplastics Identification – Tips &amp; Tricks Workshop</strong></h5><ul><li>Th, 18.12.2025 20:00 CET</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/webinar/4588">Registration</a></li></ul><p>This workshop demonstrates the workflow for analyzing microplastic samples using the Agilent 8700 Laser Direct Infrared Imaging (LDIR) system.</p></div></div></div></div></div></div>

Webinars LabRulezGCMS Week 51/2025

<p><strong>Persistent chemicals released into marine environments pose long-term and potentially irreversible risks, particularly when discharged as complex mixtures in large volumes. To address this challenge, we introduce a persistence-directed testing approach that combines environmentally relevant biodegradation experiments with nontarget analytical techniques to better characterize persistent chemical burdens.</strong></p><p>Produced waters from two offshore oil platforms in the North Sea were used as case studies. After 60 days of incubation under biotic and abiotic conditions, nontarget analyses using SPME–GC-MS and SPE–LC-HRMS identified over 600 chemicals passing quality control. Persistent compounds accounted for 4% of GC-MS detections and 32–44% of LC-HRMS detections, with several annotated as N-substituted aromatic structures. These results demonstrate the effectiveness of persistence-directed testing for revealing previously unidentified persistent chemicals and underscore the need for improved treatment of offshore produced water discharges.</p><blockquote><h4><strong>The original article</strong></h4><h4><a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/10.1021/acs.est.5c08802"><strong>Persistence-Directed Testing of Chemicals Discharged from Offshore Oil Platforms Combined with Nontargeted Analysis</strong></a></h4><p>Mette T. Møller*, Heidi Birch, Karina K. Sjøholm, Stefano Papazian, Aina C. Wennberg, Bénilde Bonnefille, Pia M. Kronsbein, Malcolm A. Kelland, Jonathan W. Martin, and Philipp Mayer</p><p>Environ. Sci. Technol. 2025, 59, 44, 24000–24011</p><p><a target="_blank" rel="noopener noreferrer" href="https://doi.org/10.1021/acs.est.5c08802">https://doi.org/10.1021/acs.est.5c08802</a></p><h6>licensed under <a target="_blank" rel="noopener noreferrer" href="https://creativecommons.org/licenses/by/4.0/"><strong>CC-BY 4.0</strong></a></h6></blockquote><p><strong>Selected sections from the article follow. Formats and hyperlinks were adapted from the original.</strong></p><p>In this study, we introduce “Persistence-Directed Testing”, a concept inspired by effect-directed analysis (EDA). In EDA toxic chemicals in complex mixtures from contaminated environments are singled out by combining fractionation procedures, biotesting, and sensitive chemical analytical methods to identify toxicants. <a href="javascript:void(0);">(13,14)</a> In persistence-directed testing, persistent chemicals in complex discharges are singled out and potentially identified by combining biodegradation tests, sensitive chemical analytical techniques, and focused data treatment schemes.</p><p>The biodegradation testing method is an advancement of a recently developed biodegradation kinetic testing method, a modified OECD 309. The method was developed for chemicals in mixtures at low concentrations, including hydrophobic and volatile chemicals. <a href="javascript:void(0);">(15,16)</a> In recent years the method has continuously been advanced from testing composed mixtures <a href="javascript:void(0);">(15)</a> to testing samples of unknown or variable composition, complex reaction products, or biological materials (UVCBs), such as petroleum mixtures and essential oils. <a href="javascript:void(0);">(17,18)</a> In the most recent progression of the method, it was used for testing the biodegradation kinetics of chemicals in complex mixtures being discharged to the environment, using native microorganisms in the receiving environment as inoculum. <a href="javascript:void(0);">(19)</a> With this method, biodegradation kinetics were successfully obtained for more than a hundred chemicals discharged from an offshore oil platform measured with solid-phase microextraction (SPME) gas chromatography-mass spectrometry (GC-MS). <a href="javascript:void(0);">(19)</a></p><p>The novelty of the persistent-directed testing in the present study is the design of the test and data treatment for persistence rather than biodegradation. This was achieved by combining a discharge sample (complex chemical mixture) and a seawater sample (native microorganisms), for determining the number, fraction, and, if possible, also the identity of those chemicals that are not degraded at the end of the test and are thus found persistent. The experiments were analyzed with both SPME GC-MS and nontarget solid-phase extraction (SPE) liquid chromatography-high-resolution mass spectrometry (LC-HRMS), in order to extend the chemical space coverage and achieve a more comprehensive persistence assessment.</p><p>Nontarget analysis (NTA) techniques have developed and advanced rapidly in recent years. <a href="javascript:void(0);">(20,21)</a> It is now possible to detect thousands of chemicals in a sample without predetermining targets. By analyzing the sample with HRMS, the exact mass of both the precursor and molecular fragments of each feature detected can be obtained, <a href="javascript:void(0);">(22)</a> which can be used for identification or annotation at various confidence levels. <a href="javascript:void(0);">(23)</a> Limitations of NTA are that exact identification (confidence level 1) and quantification is difficult and time-consuming. <a href="javascript:void(0);">(21)</a> In recent years, new developments of NTA workflows and software tools, such as in silico structure predictions <a href="javascript:void(0);">(24,25)</a> and feature-based molecular networking (FBMN), <a href="javascript:void(0);">(26,27)</a> allow increasingly more automated and higher-throughput molecular annotations (Level 2), structural elucidation (Level 3), and molecular formula assignments (Level 4). This has been successfully showcased for environmental applications. <a href="javascript:void(0);">(28−30)</a></p><p>In the present study, we combine biodegradation testing with NTA to directly enable the simultaneous persistence assessment of a large number of chemicals, while providing identification information across varying levels of confidence.</p><p>The hypotheses were: 1) environmentally relevant biodegradation tests combined with advanced analytical methods can reveal persistent chemicals in complex discharges, and 2) based on a recent feasibility study, <a href="javascript:void(0);">(19)</a> we expect a much higher fraction of persistent chemicals in produced water within the group of polar substances detectable by LC, compared to nonpolar chemicals detectable by GC. We also anticipate that NTA, combined with advanced computational workflows, can allow to reach a deeper molecular-level understanding of the persistent chemicals discovered in complex discharges.</p><h3><strong>2. Materials and Methods</strong></h3><h4><strong>2.8. Sample Preparation and Chemical Analysis</strong></h4><h5><strong>2.8.1. Solid-Phase Microextraction Coupled to GC-MS</strong></h5><p>After 60 days, test systems were transferred directly from the incubator to the GC autosampler (PAL RSI 85; CTC Analytics AG, Switzerland) without any pretreatment or conservation. Automated SPME, with a 30 μm PDMS fiber (Supelco, USA), was applied to unopened test systems by direct immersion. The SPME was thermally desorbed on the GC column (122-5562UI DB-5 ms Ultra Inert column, 60 m × 0.25 mm × 0.25 μm, Agilent), where the analytes were separated by the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=7890B"><strong>GC (7890B</strong></a>; Agilent Technologies, USA). They were then detected by the MS (<a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=5977A"><strong>5977A MSD</strong></a>; Agilent Technologies, USA), in electron ionization full-scan mode (<i>m</i>/<i>z</i> 50–500) to include a large number of nonpolar chemicals in produced water. The analytical method is described in detail in Møller et al. (2024). <a href="javascript:void(0);">(19)</a> The 1:200 dilution from both platforms was analyzed on day 60. On the following 4 days, the remaining dilutions from both platforms were analyzed, due to the number of samples and the analysis time per sample. Each GC-MS analysis run consisted of triplicate alternating biotic and abiotic test systems at one dilution from one platform, with blanks at the beginning and the end. The biotic and abiotic test systems analyzed directly after each other were used as pairs for calculating the peak area ratios.</p><h5><strong>2.8.3. LC-HRMS Analysis</strong></h5><p>Analyses by LC-HRMS for nontarget qualitative profiling were performed using a <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/744"><strong>Vanquish Horizon system</strong></a> interfaced with heated electrospray ionization (HESI) to an <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/401"><strong>Orbitrap Exploris 480</strong></a> (Thermo Fisher). Each sample was acquired twice using ionization in positive (HESI+) and negative (HESI−) modes. Clean extracts were injected (25 μL) on a <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/1952"><strong>C18 Waters Acquity column</strong></a> (UPLC BEH C18, 3.0 mm × 100 mm, 1.7 μm particle) combined with an Acquity precolumn (BEH C18, 2.1 mm × 5 mm, 1.7 μm). Reverse-phase chromatography was performed using LC-MS grade (Optima) mobile phases (A) Milli-Q water with 1 mM ammonium fluoride (NH4F), and (B) 100% MeOH. Spectral acquisition alternated between full-scan MS1 (<i>m</i>/<i>z</i> 90–1000, ∼1.5 Hz, nominal resolution 240,000 at <i>m</i>/<i>z</i> 200) and nontarget data-independent (DIA) MS2 acquisition using four sequential precursor isolation windows of 250 <i>m</i>/<i>z</i> (i.e., <i>m</i>/<i>z</i> 89–341, 339–591, 589–841, 839–1091). Additional details are presented in <a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/suppl/10.1021/acs.est.5c08802/suppl_file/es5c08802_si_001.pdf">SI 3</a>.</p><h3><strong>3. Results and Discussion</strong></h3><h4><strong>3.2. Primary Biodegradation and Persistence Assessment</strong></h4><p>Primary biodegradation and persistence were assessed at a dilution of 1:200 based on peak area ratios (biotic/abiotic) of test systems analyzed (GC) or extracted (LC) on day 60. Features were categorized as persistent, when all triplicate peak area ratios were greater than 0.5, corresponding to less than 50% biodegradation (see <a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/10.1021/acs.est.5c08802#sec2_9_2">Section 2.9.2</a>). The results for Platform B are presented in <a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/10.1021/acs.est.5c08802#fig3">Figure 3</a> (Platform A results and results including the standard error of the mean; see <a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/suppl/10.1021/acs.est.5c08802/suppl_file/es5c08802_si_001.pdf">SI 11</a>).</p><p><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/Environ_Sci_Technol_2025_59_44_24000_24011_Figure_3_Biodegradation_and_persistence_assessment_of_chemicals_in_produced_water_from_Platform_B_eab3376f2c.jpg" alt="Environ. Sci. Technol. 2025, 59, 44, 24000–24011: Figure 3. Biodegradation and persistence assessment of chemicals in produced water from Platform B at 1:200 dilution from mean (n= 3) peak area ratio. A) Features measured with GC-MS and B) Features measured with LC-HRMS. Green = primary biodegraded, yellow = ambiguous, and red = persistent (see Section 2.9.2)." srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_Environ_Sci_Technol_2025_59_44_24000_24011_Figure_3_Biodegradation_and_persistence_assessment_of_chemicals_in_produced_water_from_Platform_B_eab3376f2c.jpg 136w," sizes="100vw" width="1344" height="1544"></p><p>Assessment of the GC-MS data resulted in 3–4% persistent features for Platform A (6/144 features) and Platform B (10/279 features) (<a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/10.1021/acs.est.5c08802#fig3">Figure 3</a>A and <a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/suppl/10.1021/acs.est.5c08802/suppl_file/es5c08802_si_001.pdf">SI 11</a>), consistent with previous GC-MS results from a biodegradation experiment conducted one year earlier with produced water from Platform A, where the persistent fraction was also 4%. <a href="javascript:void(0);">(19)</a> In the present study, additional assessment performed on LC-HRMS data yielded 32% persistent features (61 of 191 features) for Platform A and 44% persistent features (183 of 416 features) for Platform B (<a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/10.1021/acs.est.5c08802#fig3">Figure 3</a>B and <a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/suppl/10.1021/acs.est.5c08802/suppl_file/es5c08802_si_001.pdf">SI 11</a>). Although the chemical space covered by the two analytical methods has only minor overlap, <a href="javascript:void(0);">(41)</a> some chemicals might still be detected by both GC-MS and LC-HRMS, as for instance was shown for the potentially persistent chemical <i>N</i>-butylbenzenesulfonamide, in our previous feasibility study. <a href="javascript:void(0);">(19)</a> The large extent of biodegradation (&gt;95%) observed in the GC-MS data set shows that microorganisms in the test systems were active (degrading).<named-content></named-content></p><p>In the GC-MS data set, 20 of the petrochemicals in the reference mixture were identified in the produced water samples from both platforms, and they were all biodegraded (benzene and toluene elute too early to be included). No spectral library matches were found for the few persistent features in the GC-MS data sets, which thus remained unidentified. In comparison, many more persistent features were detected by LC-HRMS, and the high-resolution MS data was leveraged for tentative identification of these chemicals using a combination of different workflows.</p><h4><strong>3.3. Tentative Identification of Chemicals in Produced Water (LC-HRMS)</strong></h4><h5><strong>3.3.1. Suspect Screening of Production Chemicals</strong></h5><p>In total, 55 production chemicals were included in the suspect list (<a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/suppl/10.1021/acs.est.5c08802/suppl_file/es5c08802_si_001.pdf">SI 7</a>), and 7 of these were annotated in a high-concentration sample of the produced water (1:10 dilution) at either Platform A, B, or both (accurate mass deviation &lt;0.005, as described in <a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/10.1021/acs.est.5c08802#sec2_11_1">Section 2.11.1</a>). The annotated molecular structures are presented in <a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/10.1021/acs.est.5c08802#fig4">Figure 4</a>A. These 7 production chemicals did not pass the quality control filter at 1:200 dilution since their peaks were below the blank area cutoff at this dilution. Therefore, this study cannot conclude whether these are primary biodegraded or persistent.</p><p><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/Environ_Sci_Technol_2025_59_44_24000_24011_Figure_4_Comprehensive_characterization_of_chemicals_in_produced_water_83eedbbe8e.jpg" alt="Environ. Sci. Technol. 2025, 59, 44, 24000–24011: Figure 4. Comprehensive characterization of chemicals in produced water. Examples of tentative identifications resulting from different data analysis workflows are shown. A) Suspect screening of production chemicals. B) Spectral library matching. C) Feature-Based Molecular Networking (FBMN) combined with in silico structural predictions in SIRIUS (considering maximum top-6 proposed structures). D) Molecular formula computed in SIRIUS. Suspect screening, spectral library matching, and molecular formula assignments were performed for both LC-HRMS HESI+ and HESI– data sets. The FBMN in (C) shows one example of a cluster from HESI+ (top) and one cluster from HESI– (bottom). Molecular structures highlighted in red correspond to chemicals categorized as persistent. Identification confidence levels refer to Schymanski et al. (2014). (23)" srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_Environ_Sci_Technol_2025_59_44_24000_24011_Figure_4_Comprehensive_characterization_of_chemicals_in_produced_water_83eedbbe8e.jpg 175w," sizes="100vw" width="2092" height="1871"></p><h4><strong>3.6. Persistence-Directed Testing</strong></h4><p>This study introduces persistence-directed testing and validates the hypothesis that environmentally relevant biodegradation tests combined with advanced analytical methods can reveal persistent chemicals in complex discharges. A limitation of this study is that the chemicals categorized as “biodegraded” only cover primary biodegradation and not potential persistent metabolites. More research is needed to assess persistent metabolites, e.g., by analyzing peaks that are significantly more abundant in biotic test systems compared to abiotic test systems after 60 days of incubation. If persistent metabolites are found, backtracking the parent molecule in the discharge can be challenging but is possible to approach using predicted degradation pathways, e.g., from specific mass shifts (e.g., 15.996 Da for oxygen attachment) as suggested by Tisler et al. (2022), <a href="javascript:void(0);">(46)</a> or using dedicated software such as BioTransformer (<a target="_blank" rel="noopener noreferrer" href="https://biotransformer.ca/">https://biotransformer.ca/</a>) or EnviPath (<a target="_blank" rel="noopener noreferrer" href="https://envipath.org/">https://envipath.org/</a>).</p><p>To improve the method, future studies could use sterilized inocula and discharge samples as abiotic controls. Furthermore, as analytical sensitivity increases, future studies can potentially come closer to investigating how the biodegradation process is affected by the extreme dilutions occurring in the ocean, and thereby improving environmental relevance even further.</p><p>The persistence-directed testing approach introduced in this study can be used to assess the extent of the problem of persistent chemicals in various types of discharges. An advantage of the approach is that a complex mixture of chemicals can be assessed in one biodegradation study, while the highly time-consuming work of feature identification can be narrowed down by focusing on persistent features. If persistence-directed testing approaches are adopted more widely and identification of the persistent fraction becomes easier with the very rapid development of the NTA field, it will become more and more difficult to unnoticed discharge large quantities of persistent chemicals. The approach can also lead to the identification of new groups of persistent molecules and an improved understanding of persistence in the environment.</p>

Persistence-Directed Testing of Chemicals Discharged from Offshore Oil Platforms Combined with Nontargeted Analysis

<p><strong>Our Library never stops expanding. What are the most recent contributions to LabRulezGCMS Library in the week of 15th December 2025? Check out new documents from the field of the gas phase, especially GC and GC/MS techniques!</strong></p><blockquote><p><span style="font-size:20px;">👉 </span><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library"><span style="font-size:20px;"><strong>SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT GCMS AND RELATED TECHNIQUES</strong></span></a></p></blockquote><blockquote><p><strong>👉 Need info about different analytical techniques?</strong> Peek into <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library"><strong>LabRulezLCMS</strong></a> or <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library"><strong>LabRulezICPMS</strong></a> libraries.</p></blockquote><p>This week we bring you application notes by <strong>Agilent Technologies, Shimadzu </strong>and brochure by<strong> Thermo Fisher Scientific!</strong></p><h3><strong>1. Agilent Technologies: Increased Thermal Stability of the DB‑5Q GC Column</strong></h3><p><strong>Increased signal-to-noise for trace level concentrations of controlled substances</strong></p><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_stability_gc_column_5994_8658en_agilent_4c52ae52cf.pdf"><strong>Full PDF for download</strong></a></li></ul><p>The analysis of controlled substances by gas chromatography/mass spectrometry (GC/MS) requires a high level of confidence and thus requires a method that provides optimal data quality. Identification of controlled substances relies heavily on comparison of mass spectra to commercially available spectral libraries, and increased column bleed can cause spectral interference at high temperatures. These interferences can lead to poor library matching probabilities.<sup>1-3 </sup>The <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=J%26W+5Q"><strong>Agilent J&amp;W 5Q series</strong></a> of gas chromatography columns provide the most thermally stable columns available, which helps to decrease spectral interference due to column bleed and improves data accuracy.&nbsp;</p><p>Poor thermal stability will cause an increase in the slope of the baseline as the oven temperature is increased, leading to difficult peak integrations and inaccurate quantitation. Additionally, sloped or elevated baselines can lead to a decreased response and a loss of sensitivity for analytes eluting during the oven ramp or at the method’s upper temperature limits. Several commercially available 5ms type columns were compared to the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=J%26W+DB-5Q"><strong>Agilent J&amp;W DB-5Q GC column</strong></a> to examine the impact thermal stability has on response at upper temperature limits.&nbsp;</p><h4><strong>Experimental&nbsp;</strong></h4><p>An <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=8890+GC"><strong>Agilent 8890 GC system</strong></a><strong> </strong>coupled with an <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=5977B"><strong>Agilent 5977B mass selective detector (GC/MSD)</strong></a> with an inert extractor ion source was used for acquisition of data and MassHunter 10.0 Quantitative and Qualitative Analysis software was used for data analysis.&nbsp;</p><p>A representative toxicology mixture, the Agilent GC/MS forensic toxicology checkout mixture (part number 5190-0471) was used to monitor analytical performance. Calibration standards were prepared in methanol (MeOH) at concentrations ranging from 0.1 to 3.0&nbsp;μg/mL. An internal standard mix was prepared at 10&nbsp;μg/mL from individual stocks of methamphetamine-d3, diazepam-d5, and hydrocodone-d6 all purchased from Millipore Sigma (St.&nbsp;Louis, MO).</p><h4><strong>Results and discussion&nbsp;</strong></h4><p>The testing evaluated the Agilent J&amp;W DB-5Q GC column for the analysis of controlled substances by GC/MS. The increased thermal stability of the DB-5Q is seen in the decreased baseline at higher temperatures, as seen in Figure&nbsp;1, and also provides a decrease in the slope during the oven ramping program.&nbsp;</p><p>An increase in the slope of the baseline will also decrease the signal-to-noise ratio (S/N) of an analyte but will also make integration more difficult and lead to less accurate quantitative results. Figure 2 demonstrates the comparison of the DB-5Q and the commercially available 5ms type G column, and the impact to chromatography during the oven ramp. The S/N for the analytes on the oven ramp slope are a factor of ten or greater for the DB-5Q in comparison to the 5ms type G column.</p><h4><strong>Conclusion&nbsp;</strong></h4><p>The increased thermal stability of the Agilent J&amp;W DB-5Q GC column demonstrated in this application note provides a decreased baseline at higher temperatures, which allows for an increased response for later eluting compounds at trace level concentrations. The baseline of the DB-5Q remains more consistent as the temperature is increased. This consistency allows for more accurate integration and quantitation for analytes eluting during oven ramping, in comparison to other commercially available 5ms-type columns. The robust DB-5Q column phase maintained peak shape for trace level basic compounds even when stressed with a heavy matrix and is an excellent choice for the analysis of controlled substance&nbsp;analysis.</p><h3><strong>2. Shimadzu: Quantitative Analysis of Anti-Degradant Additive (6PPD) in Tire Rubber Using Pyrolysis-GC-MS</strong></h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_01_00952_en_b95b2348e5.pdf"><strong>Full PDF for download</strong></a></li></ul><h5><strong>User Benefits</strong></h5><ul><li>The simple analysis procedure required just cutting off a sample fragment and placing it in a sample cup without pretreatment.</li><li>Utilizing a calibration standard that includes a resin solution allows for analysis under conditions that closely resemble those of samples, which improves the reliability of quantitative measurements.</li><li>With Shimadzu’s Polymer Additive Library, it is possible to acquire information on the additives of identified compounds.</li></ul><p>6PPD (N-(1,3-dimethylbutyl)-N'-phenyl-p-phenylenediamine) is an anti-degradant (anti-oxidant) additive that is used in many rubber products. Its chemical structure is shown in Fig. 1. It plays an important role in tires by preventing degradation and extending its lifespan. However, when 6PPD reacts with ozone in the atmosphere, it forms a highly toxic substance called 6PPD-quinone (6PPD-Q).&nbsp;</p><p>As an automotive tire wears, microscopic particles are released from the tire into the environment. These particles, tire road wear particles (TRWP), contain 6PPD-Q along with many other chemical substances. On rainy days, these particles are washed into rivers and other bodies of water, where they accumulate in the environment as microplastics.&nbsp;</p><p>There are serious concerns about the negative effects these microplastics have on ecosystems and the environment. 6PPDQ has been shown to induce acute mortality in Salmonidae fish, specifically coho salmon. 1)&nbsp;</p><p>Currently, there is no commercial alternative that can maintain tire stability and performance with minimal impact on the environment. Research into alternatives requires accurately assessing 6PPD levels in rubber products and objectively determining whether alternative compounds offer equivalent stability and performance while having a reduced impact on the environment.&nbsp;</p><p>This article describes using a pyrolysis gas chromatograph mass spectrometer (Py-GC-MS) system to measure 6PPD levels in tire rubber.</p><h4><strong>Analysis Process&nbsp;</strong></h4><p>ISO/TS 21396describes a method for determining the mass concentration of TRWP in soil and sediment that uses Py-GC-MS. Similar to this method, Py-GC-MS was used for the analysis; however, this article employs optimized analytical conditions. A schematic diagram of the analysis processisshown in Fig. 2. For more information on the analysis conditions and results from the evolved gas analysis (EGA-MS, <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=42&amp;search=EGA%2FPY-3030D"><strong>EGA/PY-3030D Multi-Shot Pyrolyzer AS-1020E Auto-Shot Sampler</strong></a>, Frontier Laboratories Ltd.) method described in Fig. 2, please see Application News No. 01-00901. The analysis conditions for the thermal desorption (TD)-GC/MS (<a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=1&amp;search=GCMS-QP2020+NX"><strong>GCMS-QP2020 NX</strong></a>) method used in this article are shown in Table 1. The thermal desorption temperature was chosen based on results obtained by the EGA-MS method.</p><h4><strong>Qualitative Analysis of Additive&nbsp;</strong></h4><p>The total ion current (TIC) chromatogram obtained from analyzing the tire rubber is shown in Fig. 4. A spectral library search was also performed using NIST-23 and Shimadzu’s Polymer Additives Library. The library search results for the peak that eluted at around 10.43 minutes are shown in Fig. 5. Based on the results from Shimadzu’s Polymer Additives Library, the peak was estimated to be the anti-degradant Nocrac 6C (a trade name for the chemical 6PPD).</p><h4><strong>Conclusion&nbsp;</strong></h4><p>This article presents an analysis of the additive 6PPD in tire rubber utilizing Py-GC-MS. Good results were obtained for calibration curve linearity, calibration standard repeatability, limit of quantification, and limit of detection. Shimadzu’s Polymer Additives Library was used to identify the additive.</p><h3><strong>3. Thermo Fisher Scientific: Gas chromatography analyzers for the oil &amp; gas industry: upstream to downstream</strong></h3><ul><li>Brochure</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/br_003966_gc_analyzers_trace_1610_industrial_br003966_na_en_44ad1327c6.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Gas chromatography (GC) plays a central role in the oil and gas industry, providing high-accuracy, high-speed analysis of complex hydrocarbon mixtures from upstream exploration through midstream transport to downstream refining and distribution. Across this value chain, GC supports regulatory compliance, product quality control, custody transfer, and process optimization. As the industry adapts to decarbonization goals and stricter environmental regulations, robust and automated analytical solutions have become essential for monitoring hydrocarbons, impurities, and trace components under demanding 24/7 operational conditions.</p><p>Thermo Scientific™ GC analyzers are engineered to meet these challenges, with the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/486"><strong>TRACE™ 1610 GC</strong></a> platform forming the backbone of a comprehensive portfolio of preconfigured and customizable systems. Its modular “Instant Connect” design enables rapid configuration of injectors, detectors, and valves, reducing downtime and simplifying maintenance. The platform supports multi-detector configurations—including FID, TCD, FPD, PDD, MS, and VUV—allowing a single analyzer to address a broad range of applications, from natural gas composition and BTU determination to sulfur species, fixed gases, and detailed hydrocarbon analysis .</p><p>Dedicated GC analyzer configurations are available for specific industry needs, including natural gas and natural gas liquids (NGA/NGL), refinery gas analysis (RGA), light hydrocarbons (LPG), oxygenates, aromatics (BTEX), permanent gases, and high-purity gas streams. Advanced techniques such as GC-VUV further simplify complex analyses like PIONA group-type characterization of gasoline, delivering comprehensive compositional data in a single run while reducing calibration effort and cost per sample. These systems are designed to comply with major ASTM, ISO, GPA, DIN, EN, and UOP standards, ensuring global regulatory alignment .</p><p>Complementing the hardware, <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/76"><strong>Thermo Scientific™ Chromeleon™ Chromatography Data System (CDS)</strong></a> provides an integrated informatics backbone for method control, data processing, reporting, and connectivity to LIMS platforms. This unified approach enhances data integrity, improves workflow efficiency, and enables real-time decision-making across refinery and gas processing operations. Together, Thermo Scientific GC analyzers and integrated software solutions deliver reliable, scalable, and future-ready analytics for the evolving oil and gas industry.</p>

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News from LabRulezGCMS Library - Week 51, 2025

Persistence-Directed Testing of Chemicals Discharged from Offshore Oil Platforms Combined with Nontargeted Analysis

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