Our Library never stops expanding. What are the most recent contributions to LabRulezGCMS Library in the week of 29th September 2025? Check out new documents from the field of the gas phase, especially GC and GC/MS techniques!<blockquote>👉 <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library">SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT GCMS AND RELATED TECHNIQUES</a></blockquote><blockquote>👉 Need info about different analytical techniques? Peek into <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library">LabRulezLCMS</a> or <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library">LabRulezICPMS</a> libraries.</blockquote>This week we bring you application notes by Agilent Technologies and EST Analytical, poster by Shimadzu and smart note by Thermo Fisher Scientific!<h3>1. Agilent Technologies: Equimolar Response to ASTM D5623 Relevant Sulfur Compounds</h3>Using an <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=1&amp;search=8890+GC">Agilent 8890 gas chromatograph</a> and <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=1&amp;search=8355%C2%A0SCD">8355 sulfur chemiluminescence detector (GC/SCD)</a><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_equimolar_response_astm_d5623_sulfur_compounds_5994_8562en_agilent_62a37181e4.pdf">Full PDF for download</a></li></ul>For many years, the use of a sulfur-specific detector in the petroleum industry has been invaluable for accurately identifying low levels of sulfur-containing compounds in petroleum at various stages of production.1 Many environmental and health requirements limit the amount of sulfur allowed in the final petroleum product. The presence of sulfur also has the potential to poison the catalytic processes that take place during petroleum refining.&nbsp;Along with the determination of low sulfur levels in a petroleum sample, a detector may also need to measure high sulfur levels and total sulfur content. A detector with a high linear range is essential in making both low-level and high‑level determinations of sulfur in a petroleum sample.&nbsp;In this application note, an Agilent 8355 SCD was used to measure 19 sulfur-containing compounds within a standard sample. The 8355 SCD is ideal for the widely used ASTM&nbsp;D5623 method2 because of its ability to obtain linear and equimolar responses to sulfur compounds with minimal hydrocarbon interference. When comparing the equimolar response of analytes containing different numbers of sulfur atoms, the response should be double for the analytes containing two sulfur atoms compared to those with one&nbsp;sulfur atom.&nbsp;Another advantage of the 8355 SCD is the ability to use it in tandem with an FID. This combination allows monitoring solvent elution through the GC system, assisting in the detection of the coelution of solvents with analyte peaks. These coelutions can cause peak distortion, which might be mistaken for activity issues within the GC system.<h4>Methods&nbsp;</h4><h5>Instrumentation&nbsp;</h5>Two <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=1&amp;search=8890+GC">Agilent 8890 GC systems</a> were equipped with an <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=1&amp;search=8355%C2%A0SCD">8355&nbsp;SCD</a>. Both GC/SCD systems were run in the same manner to confirm equimolar results. A third GC system was also configured with a tandem flame ionization detector sulfur chemiluminescence detector (FID/SCD) to allow the determination of the solvent peak elution from the system. This third system also served as another confirmation of the equimolar results that were obtained from the other two GC/SCD systems. Sample introduction for all systems was completed with an Agilent <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=1&amp;search=7693A+automatic+liquid+sampler">7693A automatic liquid sampler</a> with a 5 µL syringe. The sample volume for each injection was 1.0 µL. All analyses were performed with a split/splitless inlet in split mode.&nbsp;The GC/SCD parameters are provided in Table 1. Note that an Agilent DB-Sulfur SCD GC column (part number G3903-63002) was used in this study because of the low column bleed and excellent inertness and performance for sulfur compound analysis. When using the SCD, be aware that stationary phase bleed from the GC column can lead to fouling of the ceramic tubes within the detector. This phenomenon can cause poor SCD performance, such as decreased sensitivity, and may require more frequent maintenance. Proper GC column selection (such as the DB-Sulfur column) is important to ensure lower column bleed into the detector and will reduce fouling of ceramic tubes, reducing instrument downtime.<h4>Results and discussion</h4><h5>Use of GC/FID for solvent elution determination&nbsp;</h5>Determination of the solvent peak elution can be a challenge when using a sulfur-selective detector such as the SCD. Many times, the large, fronting solvent peak may coelute with analytes of interest, causing distortion of the analyte peak shape (peak tailing, fronting, or broadening) and poor chromatographic separation. This poor peak shape, caused by column overloading, can be mistaken for activity issues in the system or hydrocarbon interferences, leading to unnecessary troubleshooting or inlet/column maintenance. Determination of the solvent peak elution time is recommended to ensure that coelution does not occur with any of the analytes of interest. To confirm the solvent elution time, a tandem GC/FID/SCD system was used. The GC/FID/SCD system puts the FID in-line before the SCD analysis, allowing the user to obtain both FID and SCD signals from a single injection, thus confirming the solvent retention time and determining any solvent/analyte coelutions.&nbsp;<h4>Conclusion&nbsp;</h4>The Agilent 8355 sulfur chemiluminescence detector, paired with an Agilent 8890 GC, was evaluated by analyzing 19&nbsp;sulfur‑containing compounds relevant to ASTM D5623. The SCD met the specifications of the test method, including an equimolar response to the analyzed sulfur compounds and a wide range of linearity to a sulfur-containing standard. The 8355 SCD shows excellent area reproducibility, and when used in tandem with a flame ionization detector, the system can aid in the determination of solvent peak elution through the GC system.<h3>2. EST Analytical: Reducing Carryover in Environmental Water Samples</h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/Purge_and_Trap_Reducing_Carryover_in_Environmental_Water_Samples_6e5ba0a008.pdf">Full PDF for download</a></li></ul>In order to mitigate carryover, many environmental labs resort to running sample dilutions or adding blank samples after a highly contaminated sample. Both of these solutions are not ideal and can lead to a loss of analyte detection when diluting or a loss of profits when blank samples need to be run.Since, the primary source of carryover for water samples is the sparge vessel, purge and trap manufactures have incorporated a rinsing step in which the sparge vessel is “washed” with hot water in order to clean up the volatile compounds that may still reside in the sparge vessel. Expanding on the idea of limiting volatile compounds in the sparge vessel, EST Analytical developed a patented process of heating the sparge vessel during the bake step of the purge and trap process (Patent Number: US 8,075,842 B1) . This engineering innovation essentially performs two bakes; as a result both the trap and the sparge vessel are “cleaned” at the same time. No other concentrator is or can be engineered to do this.<h4>Experimental</h4>The sampling system used for this study was the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/2160">EST Analytical Evolution concentrator</a> and the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/2159">Centurion WS autosampler</a>. The concentrator was affixed with a Vocarb 3000 trap and connected to an <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=1&amp;search=7890A">Agilent 7890A GC </a>and <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=1&amp;search=5975C">5975C inert XL MS</a>. The GC was configured with a <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=9&amp;search=Rxi-624+Sil+MS">Restek Rxi-624 Sil</a> MS 30m x 0.25mm x 1.4µm column. Refer to Table 1 for the sampling method parameters and Table 2 for GC/MS parameters.<h4>Conclusions</h4>The Evolution purge and trap concentrator with its patented technique of heating the sparge vessel during the bake process proved to reduce carryover by almost half when comparing with hot water rinses alone. The advantages of reduced carryover are many. Primary among them is the ability to run more samples during the twelve hour tune window. This increase in productivity translates to more laboratory profits and better use of instrument time.<h3>3. Shimadzu / AOAC: Analysis of PFAS in juice using Head-Space Solid Phase Microextraction-Gas Chromatography/Mass Spectrometry (HS-SPME GCMS)</h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/aoac_2025_t010_9967ebebff.pdf">Full PDF for download</a></li></ul>PFAS contaminate water and food through packaging that can leach volatile PFAS from plastics and inks or coatings. This work developed a headspace SPME GCMS method to analyze six volatile PFAS classes in juices. The United States Food and Drug Administration has tested for PFAS in a broad range of foods and beverages as part of its Total Diet Study. Juice matrices differ in flavor, sugar, as well as manufacturing practices, and packaging, with the latter two potentially introducing PFAS contamination. The former differences between products can impact PFAS detection.<h4>Materials and Methods</h4>The SPME method used in this study is based on a method published by Bach et.al. (2016). An HS-SPME method is used to improve method performance when analyzing complex aqueous samples over direct immersion. The optimized parameters of the instrument method for the targeted PFAS are listed in table 1.<h4>Conclusion&nbsp;</h4>The <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=3&amp;search=GCMS-TQ8040+NX">Shimadzu GCMS-TQ8040 NX triple quadrupole instrument</a>, configured with an <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=3&amp;search=AOC-6000+Plus+SPME">AOC-6000 Plus SPME</a> unit, was used to measure PFAS in different juice samples. Without isotope dilution, matrix effects caused recoveries to fall outside of acceptable criteria. Method blanks showed no detectable PFAS, and calibration demonstrated excellent linearity (R² ≥ 0.993). This HS-SPME GCMS-TQ8040 NX method demonstrated quantitative capability for analyzing nanogram-per-liter PFAS compounds in complex juice matrices. This application highlights a simple, fast, robust, precise, and accurate workflow for measuring volatile PFAS in challenging matrices.<h3>4. Thermo Fisher Scientific: Safe use of carrier hydrogen for air monitoring with Multi-Gas TD-GC-MS</h3><ul><li>Other document (smart note)</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/sn_003958_gc_single_quad_gc_ms_isq_7610_environmental_sn003958_na_en_8216fc7021.pdf">Full PDF for download</a></li></ul>Monitoring volatile organic air compounds, also known as hazardous air pollutants (HAPs), is crucial for maintaining air quality in urban and industrial environments due to their significant health risks. The growing concerns about these potentially dangerous volatile organic compounds in ambient air, particularly in urban areas and from industrial emissions, have led to the development of numerous national and international regulations. The use of Thermal Desorption (TD) coupled with GC-MS is the analytical technique of choice to enrich volatile organic compounds from air and quantify them at trace levels.1 In gas chromatography, the choice of carrier gas is pivotal for the separation and detection of VOCs. Helium has traditionally been the preferred carrier gas for analyzing volatile organic air toxics due to its inertness and performance benefits. However, hydrogen is becoming increasingly popular due to economic and supply considerations. Each carrier gas has unique advantages and challenges, and the choice should be guided by specific analytical requirements, cost constraints, and safety protocols. As the demand for sustainable and cost-effective solutions grows, hydrogen is expected to play a more significant role in monitoring hazardous air pollutants in urban and industrial settings.Thermal Desorption is an established way to analyze VOCs in a wide variety of sample types. This smart note highlights the use of the new Multi-Gas TD system (Markes International) that allows a safe use of carrier hydrogen for the analysis of VOCs in air, enhancing operational flexibility and supporting more sustainable laboratory practices.&nbsp;<h4>Experimental&nbsp;</h4>In this study, <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=7&amp;search=TD100-xr">Markes TD100-xr™ Multi-Gas system</a>, coupled with the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/486">Thermo Scientific™ TRACE™ 1610 gas chromatograph</a> and <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/484">Thermo Scientific™ ISQ™ 7610 single quadrupole mass spectrometer,</a> was employed to accurately detect and quantify compounds for effective air monitoring. This combination leverages several technological advancements to optimize analytical performance and operational efficiency.The comparison between helium and hydrogen carrier gas was carried out using the same analytical column. The method conditions for all analytes could be easily transferred. Flow rates were adjusted using the split ratio calculator available in the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/76">Thermo Scientific™ Chromeleon™ Chromatography Data System (CDS)</a> Instrument Method Wizard (Figure 1) to maintain the same split level and therefore the same amount of transferred sample. A further factor facilitating rapid adoption of hydrogen carrier gas in laboratories is that existing columns and consumables can be used without restrictions.<h4>Conclusion&nbsp;</h4>The use of the Markes TD100-xr Multi-Gas system combined with the ISQ 7610 GC-MS for the analysis of VOC in air allows for a safe use of carrier hydrogen, making it a viable alternative to helium and offering an effective solution for laboratories facing the challenges of helium scarcity and rising costs, while maintaining the accuracy and reliability of VOC detection and quantification.&nbsp;<ul><li>The comparative analysis clearly confirmed that using hydrogen carrier gas in gas chromatography offers substantial benefits over helium. The significant reduction in retention time, as shown by the 60% decrease for 1,2,3-trichlorobenzene, leads to faster analysis without compromising the separation efficiency.&nbsp;</li><li>Enabling shorter analysis time, hydrogen enhances laboratory productivity, reduces costs, and contributes to more sustainable practices.&nbsp;</li><li>The results also indicate that both helium and hydrogen can be used effectively as carrier gases without impacting the response linearity for the VOC compounds under evaluation. Laboratories can confidently use hydrogen as an alternative to helium for quantitative analysis, ensuring accurate and reliable analytical results.</li><li>When using multiple carrier gases, the ISQ 7610 NeverVent technology is key to easily switching from helium to hydrogen and back to helium with no venting required, making this operation very quick and safe.&nbsp;</li></ul>In conclusion, coupling the Markes TD100-xr Multi-Gas system with the ISQ 7610 single quadrupole GC-MS offers a robust and flexible solution for air monitoring. This integration enhances operational efficiency, reduces costs, and maintains high data integrity, making it an invaluable tool for modern analytical laboratories.

News from LabRulezGCMS Library - Week 40, 2025

Our Library never stops expanding. What are the most recent contributions to LabRulezGCMS Library in the week of 6th October 2025? Check out new documents from the field of the gas phase, especially GC and GC/MS techniques!<blockquote>👉 <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library">SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT GCMS AND RELATED TECHNIQUES</a></blockquote><blockquote>👉 Need info about different analytical techniques? Peek into <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library">LabRulezLCMS</a> or <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library">LabRulezICPMS</a> libraries.</blockquote>This week we bring you poster by Agilent Technologies / AOAC, application notes by EST Analytical and Shimadzu and brochure by Thermo Fisher Scientific!<h3>1. Agilent Technologies / AOAC: Method Translation for the Analysis of Vanilla Extracts Using a Compact, Single Channel GC-FID and Carrier Gas Switching Module</h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/ps_vanilla_single_channel_gcfid_carrier_gas_aoac_2025_w020_en_agilent_17c7d568c9.pdf">Full PDF for download</a></li></ul>Vanilla is a flavor variety that has been heavily impacted by changes in consumer habits as well as by supply and demand of vanilla beans used to produce high-quality vanilla extracts. Unfortunately, these market conditions, increase the likelihood of adulteration in vanilla extracts by use of aroma chemicals that are not naturally occurring. Common adulterants are coumarin (C), ethyl vanillin (EV), eugenol (E), and guaiacol (G).2,3 Adulteration impacts the standard of identity for vanilla extracts established by the U.S. FDA; therefore, flavor companies rely on QC labs to implement reliable and sensitive analysis techniques for screening incoming raw ingredients against expected purity standards before the ingredient can enter a flavor formula on the manufacturing floor. Screening is typically executed with gas chromatography (GC)- based methods adapted from those used in a R&amp;D lab. However, differences in column length, diameter, and phase can make it seem challenging to harmonize GC methods across the R&amp;D and QC functions within a company due to the different analysis objectives of the respective laboratories.&nbsp;<h4>Experimental Goals</h4><ul><li>Demonstrate the ease of the Agilent Method Translator in harmonizing GC methods for multiple columns and gases&nbsp;</li><li>Establish method precision, linearity, and resolution on standards of vanilla-like adulterants using the translated methods&nbsp;</li><li>Successfully showcase the method translation using store-bought extracts to verify the integrity of the fastest GC method on samples containing matrix&nbsp;</li><li>Screen for and quantify any vanilla adulterants in the samples of vanilla extracts with the goal of detecting no adulterants using the fastest GC method.</li></ul><h4>Experimental&nbsp;</h4><ul><li>GC System: <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=8850+GC">Agilent 8850 GC</a> with <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=7693A+Automatic+Liquid+Sampler">7693A Automatic Liquid Sampler</a></li></ul><h4>Conclusions</h4><h5>Method Translation</h5><ul><li>The method translator tool provided an easy conversion of a 50-minute-long method to one that is &lt; 5 minutes resulting in a speed gain of 10-fold and 14-fold, for He and H2 carrier gases, respectively (Figures 2 and 3)&nbsp;</li><li>Resolution of analytes were &gt;4 on the 60 m and &gt;3.5 on the 10 m DB-1 columns (Table 2)</li><li>Precision was &lt;1.85% RSD and &lt;2.5% RSD for He and H2 carrier, respectively (Table 3)</li><li>Linearity was demonstrated from 10 ppm to 100,000 ppm for He and H2 carrier with R2 ranging from 0.9997 to 1.0000&nbsp;</li></ul><h5>Carrier Gas Switching</h5><ul><li>He and H2 carrier gases were alternated line by line in a sequence table for increased analytical efficiency and higher throughput while demonstrating the flexibility the helium conservation module provides its users while also eliminating manual changes to plumbed gases at the GC EPC Module.</li></ul><h3>2. EST Analytical: Optimizing 8260 Sample Throughput - Solutions for the Determination of Bromomethane by Purge and Trap</h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/Purge_and_Trap_Solutions_for_the_Determination_and_Stability_of_Bromomethane_by_P_and_T_App_Note_Rev_2_177c75d029.pdf">Full PDF for download</a></li></ul>The United States Environmental Protection Agency’s (USEPA) Method 8260 has an extensive list of compounds of interest. In order to purge and trap these analytes, there needs to be an analytical trap able to trap these compounds and desorb them to the Gas Chromatograph/Mass Spectrometer (GC/MS) both accurately and efficiently. Due to the broad range of compounds on the Method 8260 list, there are many issues to take into account. Purge efficiency, molecular weight, volatility, and water are among the most problematic issues. The purge and trap concentrator and analytical trap must be able to account for all of these concerns.&nbsp;The most commonly used analytical trap is the Vocarb® 3000 due to its ability to trap and desorb the extensive analyte list both effectively and correctly. However, the Vocarb® 3000 trap is not without its drawbacks. One of which is Bromomethane degradation in the trap over time. This application will examine the Vocarb® 3000 and a custom trap along with the optimum trap temperature parameters for the stability of Bromomethane.&nbsp;<h4>Experimental</h4>The purge and trap concentrator used for this study was the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/2160">EST Analytical Evolution</a>. The <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/2159">Centurion Water and Soil autosampler</a> equipped with the syringe option was employed as the autosampler. Separation and analysis of the volatile compounds was performed by the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=1&amp;search=7890A">Agilent 7890A Gas Chromatograph (GC) </a>and <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=5977B">5977B Mass Spectrometer</a> (MS). The GC was configured with a <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=9&amp;search=Rxi-624+Sil+MS">Restek Rxi624 Sil MS</a> 30m x 0.25mm x 1.4µm column. The purge and trap parameters and analytical traps used for this study are listed in Tables 1 and 2 while Table 3 details the GC/MS parameters.<h4>Conclusions</h4>Initially, all of the traps and heating parameters used in the EST Analytical Evolution met USEPA method 8260 requirements and could be used in the laboratory. However, the custom trap and the higher temperature desorb and bake showed a lower response when compared to using a lower temperature desorb and bake. Furthermore, over time, the custom trap and higher temperature desorb and bake displayed lower recoveries of Bromomethane which could in turn affect the continuing calibration standards. The Vocarb® 3000 trap with the lower temperature desorb and bake proved to be the optimum method for sampling USEPA Method 8260 compounds. The technique met all of the method requirements and exhibited the best response and stability not only for Bromomethane but also for the rest of the extensive compound list.<h3>3. Shimadzu: Quantitative Analysis of Furan and Alkylfurans in Processed Food Using Headspace GC-MS</h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_01_00906_en_878a49b98e.pdf">Full PDF for download</a></li></ul>Furan and alkylfurans are aromatic compounds with a fivemembered ring structure. Furan and some alkylfurans, such as 2-methylfuran, 3-methylfuran, and 2,5-methylfuran (furan with a hydrocarbon chain attached), are found in processed food. They are generated through a variety of pathways during heat treatment of the food. Some countries have studied these compounds and concluded they are a health concern. 1) At present, no country has set permissible levels for furan or alkylfurans in food. But since they are harmful substances that are generated unintentionally during the processing of food, analyzing them is becoming increasingly important. In this Application News, the levels of furan and alkylfurans in commercially available processed food were measured.<h4>Equipment&nbsp;</h4>The <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=1&amp;search=GCMS-QP2050">GCMS-QP2050</a> gas chromatograph mass spectrometer has a compact design for a smaller installation footprint. When combined with the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=1&amp;search=HS-20+NX">HS-20 NX headspace sampler</a>, the GCMSQP2050 can simply and accurately measure furan and alkylfuran levels in processed food. The DuraEase ion source, which is specifically designed for durability and ease of maintenance, also providesreduced maintenance requirements.<h4>Conclusion&nbsp;</h4>In this Application News, headspace GC-MS analysis was used to measure levels of furan and alkylfurans in processed food. Analysis of standard samples produced good results in terms of separation, calibration curve linearity, and repeatability. Analyzing food samples and comparing the results obtained by the external standard method and the standard addition method showed that the matrix effects differed depending on the sample.<h3>4. Thermo Fisher Scientific: Everything You Need in a GC Detector: VGA-100 Gas Chromatography Detector for TRACE 1600 Series GC</h3><ul><li>Brochure</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/br_003592_gc_vuv_detector_vga_100_isomers_br003592_na_en_0a48830aff.pdf">Full PDF for download</a></li></ul><h4>Performance synergy—the VGA-100 detector and the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/483">TRACE 1600 Series GC</a>&nbsp;</h4>VUV absorbance and gas chromatography offer a perfect match, joining insights on light absorption in the VUV range with each compound’s unique gas phase absorption features. The innovative VUV absorption technology of the VGA-100, combined with the robust and reliable performance of the Thermo Scientific™ TRACE™ 1600 Series gas chromatograph, offers a powerful analytical solution to support timecritical laboratory demands.&nbsp;Harnessing breakthrough gas chromatography technology, VGA-100 provides unmatched precision and data quality with faster results and higher sample volume. Experience analytical insights with a system designed for ease of use that delivers accurate, reportable results across a diverse range of industries.<h4>Explore the benefits of VUV technology&nbsp;</h4>The unique capabilities of the VGA-100 detector for the TRACE 1600 Series GC help solve common challenges, such as correct isomer identification, poor selectivity, long method run times, analyte co-elution, burdensome data processing and analysis, and method scalability to production environments.&nbsp;<h5>Expand detectable compounds.&nbsp;</h5>Access to a wider range of analytes with enhanced sensitivity towards impurities as well as accurate sample profiling, thanks to the combined universal and selective response of the VGA-100 detector.&nbsp;<h5>Unambiguous identification.&nbsp;</h5>The VGA-100 universal mass-sensitive detector delivers comprehensive data for robust analysis. Data provided in 3D (time, wavelengths, and intensity) supports reliable identification through spectra that can be matched to a dedicated library, including isomers discrimination.&nbsp;<h5>Ease of use and maintenance.&nbsp;</h5>Robust and easy to set up and operate, the VGA‑100 requires minimal maintenance, with no vacuum pumps required. An intuitive design supports high demands for throughput and compliance, supporting the needs of both research and quality control laboratories.&nbsp;<h5>Faster analysis.&nbsp;</h5>Obtain rapid and accurate results with the advanced capabilities of VUV technology, complemented by the fast and efficient chromatographic separation of the TRACE 1600 Series GC.&nbsp;<h5>VUV Analyze Software for push-button simplicity&nbsp;</h5>The advanced post-acquisition processing capabilities of VUV Analyze™ Software (VUV Analytics, Inc.) allows laboratories to generate meaningful results with just the push of a button. This cutting-edge software platform swiftly analyzes complex chromatographic and spectral data, delivering method-specific results and reports. By automating the analysis process, VUV Analyze Software significantly streamlines and speeds up each run while minimizing errors, leading to greater confidence in results.

News from LabRulezGCMS Library - Week 41, 2025

<h4>Abstract&nbsp;</h4>Environmental laboratories are always searching for techniques to increase productivity. However, environmental methods demand a large amount of background information in order to ensure sampling and analysis is compliant. The determination of <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=45&amp;search=VOC">Volatile Organic Compounds (VOCs) </a>in the United States Environmental Protection Agency (USEPA) <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=45&amp;search=Method+8260">Method 8260</a> encompasses many different matrices and in doing so has numerous sampling, quality control, and calibration requirements. The matrices of Method 8260 samples can also vary from air to sludge and from clean to extremely contaminated. Furthermore, the method has an extensive calibration range. All of these factors play into the complexity of sampling and analysis thus, creating ways to streamline sampling while still maintaining sample integrity and method compliance is always of interest to environmental laboratories.<h4>Introduction</h4>In order to run Method 8260 samples, a bromofluorobenzene (BFB) tune standard, matrix blank, calibration standard, and laboratory control standard all have to be run and pass method requirements every twelve hours. With the exception of the BFB standard, the other standards and blank matrices have to correspond to the samples to be analyzed. Due to this constraint, the analyst is required to run another three samples if the matrix is changed within the twelve hour time window. Moreover, the calibration must also match the sample matrix. These requirements are very time consuming and can limit laboratory profits. This application note will demonstrate a patented automated water sampling mode using the soil sampling station of the autosampler thus eliminating the need to have separate calibrations and standards for waters and soils.&nbsp;<h4>Discussion</h4>There are a number or techniques that can enable an analyst to save time in an environmental lab. Analysts can decrease analytical trap bake times, change sample purge time and flow, utilize a dual sampling system for one GC/MS, etc. However, one of the most basic ways to save time is by reducing the number of required curves and standards needed.EST Analytical has designed a patented, automated water sampling mode that will allow environmental laboratories to run water samples in the soil mode. Thus, water and soil curves, standards, blanks and samples can use the same sampling parameters. (See steps 1, 2, and 3 below). This innovative sampling mode would eliminate the need to have separate curves, standards, etc. for soils and waters, thus saving laboratories time and money. Please note that this procedure may only be used with auditor approval.<img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/EST_Analytical_Experimental_9f34a58017.jpg" alt="EST Analytical: Sampling" srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_EST_Analytical_Experimental_9f34a58017.jpg 245w," sizes="100vw" width="1386" height="861"><h4>Experimental</h4>The sampling system used for this study was the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/2159">EST Analytical Centurion WS autosampler</a> and <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/2160">Evolution concentrator</a>. The concentrator was affixed with a Vocarb 3000 trap and connected to an <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=7890A">Agilent 7890A GC</a> and <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=5975C">5975 inert XL MS</a>. The GC was configured with a <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=7&amp;search=Restek+Rxi-624+Sil+MS">Restek Rxi-624 Sil MS</a> 30m x 0.25mm x 1.4µm column. The experiments were run using the extraction mode of the Centurion WS. Sampling method parameters and GC/MS parameters are listed below.<h5>Purge and Trap Parameters</h5><ul><li>Concentrator: EST Evolution</li><li>Trap type: Vocarb 3000</li><li>Valve oven temperature: 150 °C</li><li>Transfer line temperature: 150 °C</li><li>Trap temperature: 35 °C</li><li>Moisture Reduction Trap (MoRT) temperature: 39 °C</li><li>Purge time: 11 min</li><li>Purge flow: 40 mL/min</li><li>Dry purge Temp.: Ambient</li><li>Dry Purge Flow: 40mL/min</li><li>Dry Purge Time: 1.0 min &nbsp;</li><li>Desorb pressure Control: ON</li><li>Desorb Pressure: 5psi</li><li>Desorb time: 0.5 min</li><li>Desorb preheat delay: 5 sec</li><li>Desorb temperature: 260 °C</li><li>MoRT bake temperature: 230 °C</li><li>Bake temperature: 270 °C</li><li>Sparge vessel bake temperature: 120 °C</li><li>Bake time: 8 min</li><li>Bake flow: 40 mL/min</li></ul><h5>Auto-Sampler (EST Centurion WS):</h5><ul><li>Sample type: Water Extraction</li><li>Sample Fill Mode: Syringe</li><li>Sample Volume: 10mL</li><li>IS Volume: 5µl</li><li>Needle Rinse Time: 20 sec</li><li>Needle Sweep Time: 20 sec</li><li>Concentrator Desorb Time: 0.5 min</li><li>Syringe Rinse: On/12mL</li><li>Number of Syringe Rinses: 2</li><li>Sparge Rinse Time: Off</li><li>Water Heater Temp.: 85°C</li></ul><h5>GC/MS Parameters</h5><ul><li>System: Agilent 7890/5975 inert XL</li><li>Inlet: Split mode, 200 °C, 40:1 split ratio, 12.153 psi head pressure</li><li>Column: Restek Rxi-624Sil MS, 30 m × 0.25 mm × 1.4 µm</li><li>Oven program: 45 °C (1 min) → ramp 15 °C/min → 220 °C, hold 1.3 min</li><li>Column flow rate: 1 mL/min helium</li><li>Total flow: 44 mL/min</li><li>Source temperature: 230 °C</li><li>Quadrupole temperature: 150 °C</li><li>Transfer line temperature: 180 °C</li><li>Scan range: m/z 35–265, 3.12 scans/sec</li><li>Solvent delay: 0.7 min</li></ul>The USEPA Method 8260 standards were acquired from Restek. The linear range of the water extraction experiment was established by running a nine point calibration curve with a range of 0.5 to 200ppb. Method detection limits were also established for each compound by examining seven replicate standards of the low calibration point. Finally, precision and accuracy were determined by running seven replicate midpoint standards. Figure 1 displays a 50ppb Method 8260 standard chromatogram of a water sample run in soil mode and experimental results are listed in Table 1.<img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/EST_Analytical_Obrazek_1_Chromatogram_50_ppb_vzorku_vody_analyzovaneho_v_rezimu_puda_55ffcb4ba3.jpg" alt="EST Analytical: Figure 1: 50ppb Chromatogram of a Water Sample Run in Soil Mode" srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_EST_Analytical_Obrazek_1_Chromatogram_50_ppb_vzorku_vody_analyzovaneho_v_rezimu_puda_55ffcb4ba3.jpg 245w," sizes="100vw" width="1444" height="514"><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/EST_Analytical_Tabulka_3_Vysledky_experimentu_cast_1_7cadc58cda.jpg" alt="EST Analytical: Table 3: Experimental Results_part 1" srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_EST_Analytical_Tabulka_3_Vysledky_experimentu_cast_1_7cadc58cda.jpg 215w," sizes="100vw" width="1568" height="1143"><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/EST_Analytical_Tabulka_3_Vysledky_experimentu_cast_2_f676814e52.jpg" alt="EST Analytical: Table 3: Experimental Results_Part 2" srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_EST_Analytical_Tabulka_3_Vysledky_experimentu_cast_2_f676814e52.jpg 245w," sizes="100vw" width="1571" height="616"><h4>Conclusion</h4>The patented sampling process of the Centurion WS proved to be a reliable and accurate sampling method for running water samples in the soil mode. The curve linearity and method detection limits both met USEPA Method 8260 requirements, and the precision and accuracy results were excellent. The water extraction option offered with the Centurion WS will save laboratories time and money because only one set of standards, curves, etc. is required for both water and soil samples.

A Single Calibration Method for Water AND Soil Samples Performing EPA Method 8260

Our Library never stops expanding. What are the most recent contributions to LabRulezGCMS Library in the week of 13th October 2025? Check out new documents from the field of the gas phase, especially GC and GC/MS techniques!<blockquote>👉 <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library">SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT GCMS AND RELATED TECHNIQUES</a></blockquote><blockquote>👉 Need info about different analytical techniques? Peek into <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library">LabRulezLCMS</a> or <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library">LabRulezICPMS</a> libraries.</blockquote>This week we bring you poster by Agilent Technologies / AOAC and application notes by EST Analytical, Shimadzu and Thermo Fisher Scientific!<h3>1. Agilent Technologies / AOAC: Analysis of Pesticides in Spices with Hydrogen Carrier Gas</h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/ps_pesticides_hydrogen_carrier_gas_aoac_2025_w007_en_agilent_280dd876d5.pdf">Full PDF for download</a></li></ul>Spices are considered as one of the most challenging matrices for analysis of pesticides. Usually, the sample analysis involves 5-10 fold dilution to reduce the matrix load. Thus, lower instrument detection limits need to be achieved. Use of hydrogen as carrier gas can further pose changes in terms of sensitivity. This work describes the suitability of the hydroinert and HES ion source to achieve the required sensitivity. Samples were extracted using QuEChERS based approach followed by dispersive cleanup. Linearity was evaluated against matrix matched standards within the range of 0.5-50 ng/mL. Correlation coefficient (r2) for calibration ranging between 0.5 -50 ng/mL was found above 0.95. Precision study was carried out by injecting 6 replicates of pre-spiked samples at 10 ng/g. The average relative standard deviation (%RSD) was &lt;20% with recoveries ranging from 72-125%. The advantages of the method include utilization of same retention time MRMs and collision energies. This allowed for easy transition from helium to hydrogen carrier gas.<h4>Experimental</h4>An Agilent <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=8890+GC">8890 GC</a> coupled to a 7000 (with HydroInert source) / <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=7010+Triple+Quadrupole+GC%2FMS">7010 Triple Quadrupole GC/MS</a> system equipped with High Efficiency Source (HES) was used. The GC system was equipped with a MultiMode Inlet (MMI) with air cooling and a back flushing system based on a Purged Ultimate Union controlled by a PSD module.<h4>Results and Discussion&nbsp;</h4>The oven temperature program used with H2 as the carrier gas was maintained identical to that used with He. The analytical method originally optimized for a 20- minute runtime using He was successfully adapted for H2. This ensured preservation of chromatographic resolution and retention time fidelity across carrier gas substitution, as evident from the elution order shown in Figure 3. The chromatograms indicate presence of high matrix load at initial 7 mins for all the spices. At RT 10-13 min, matrix load of and chilli was high. The matrix load from black pepper was very high throughout the runtime. Backflush of 7 min was used to remove the matrix.&nbsp;Transitioning from He to H2 can often lead to reactions at the ion source resulting in spectral changes when compared with He. Therefore, EI sources with reduced or eliminated source reactivity such as HydroInert and HES is essential to minimize or prevent the undesirable insource reactions when using hydrogen. The tested mixture of pesticides were compared against the NIST library to ensure spectral fidelity. As evident form Figure 5, the library match percentages were acceptable and this the existing MRM database could be used for acquisition in MRM mode, without the requirement of any additional MRM development.<h4>Conclusions</h4>Agilent GC/TQ systems with HydroInert and HES sources delivered consistent sensitivity and spectral fidelity using hydrogen carrier gas, without re-optimizing MRM transitions or collision energies. Retention times and elution order were preserved across complex spice matrices. The systems achieved LOQs of 2.5 to 5 ppb after five-fold dilution, even in heavily loaded matrices like black pepper, confirming reliable quantitation in high-background spice samples.<h3>2. EST Analytical: A Single Calibration Method for Water AND Soil Samples Performing EPA Method 8260</h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/Purge_and_Trap_A_Single_Calibration_Method_for_Water_AND_Soil_Samples_Performing_EPA_Method_8260_27f8b93aad.pdf">Full PDF for download</a></li></ul>In order to run Method 8260 samples, a bromofluorobenzene (BFB) tune standard, matrix blank, calibration standard, and laboratory control standard all have to be run and pass method requirements every twelve hours. With the exception of the BFB standard, the other standards and blank matrices have to correspond to the samples to be analyzed. Due to this constraint, the analyst is required to run another three samples if the matrix is changed within the twelve hour time window. Moreover, the calibration must also match the sample matrix. These requirements are very time consuming and can limit laboratory profits. This application note will demonstrate a patented automated water sampling mode using the soil sampling station of the autosampler thus eliminating the need to have separate calibrations and standards for waters and soils.<h4>Experimental</h4>The sampling system used for this study was the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/2159">EST Analytical Centurion WS autosampler</a> and <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/2160">Evolution concentrator</a>. The concentrator was affixed with a Vocarb 3000 trap and connected to an <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=1&amp;search=7890A">Agilent 7890A GC</a> and <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?search=5975">5975 inert XL MS</a>. The GC was configured with a <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=9&amp;search=Rxi-624+Sil+MS">Restek Rxi-624 Sil MS </a>30m x 0.25mm x 1.4µm column. The experiments were run using the extraction mode of the Centurion WS. Refer to Table 1 for the sampling method parameters and Table 2 for GC/MS parameters.<h4>Conclusion</h4>The patented sampling process of the Centurion WS proved to be a reliable and accurate sampling method for running water samples in the soil mode. The curve linearity and method detection limits both met USEPA Method 8260 requirements, and the precision and accuracy results were excellent. The water extraction option offered with the Centurion WS will save laboratories time and money because only one set of standards, curves, etc. is required for both water and soil samples.<h3>3. Shimadzu: Measurement of Volatile Organic Compounds in Water by Headspace GC-MS with Nitrogen Carrier Gas</h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_01_00907_en_077ab0a675.pdf">Full PDF for download</a></li></ul>Due to the health issues associated with volatile organic compounds (VOCs), standards and regulations are established for VOC levels in water. VOCs are preferably measured by methods that involve simple sample pretreatment, and headspace GC-MS is one of these methods commonly used to measure VOC levels. GC-MS is normally performed with helium carrier gas, but helium gas could require more cost and lead time to obtain for analytical use every year. There is a need for a GC-MS analysis method that can be performed using relatively inexpensive and readily available nitrogen carrier gas. While nitrogen carrier gas results in inferior analytical sensitivity compared with helium carrier gas, trap mode sampling can salvage the reduction of the sensitivity. This Application News presents an example measurement of VOCs in water using nitrogen carrier gas performed on the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=1&amp;search=GCMS-QP2050">GCMS-QP2050</a> gas chromatograph mass spectrometer and the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=1&amp;search=HS-20+NX">HS-20 NX headspace sampler</a> in trap mode.<h4>Samples and Analysis Conditions&nbsp;</h4>Standard solutions were prepared by diluting 25 standard VOC mixture in methanol to 1, 2.5, 5, 10, 25, 50, 100, and 250 mg/L. The standard solutions were combined with internal standards 1,4-dioxane-d8 at 100 mg/L, fluorobenzene at 12.5 mg/L, and pbromofluorobenzene at 12.5 mg/L.<ul><li>GC-MS: <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=1&amp;search=GCMS-QP2050">GCMS-QP2050</a></li><li>Head Space Sampler: <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=1&amp;search=HS-20+NX">HS-20 NX</a></li></ul><h4>Conclusion&nbsp;</h4>VOC levels in water were measured using an HS-20 NX in trap mode and a GCMS-QP2050 with nitrogen carrier gas. Trap mode allowed VOCs to be measured in water with a high degree of sensitivity, even with nitrogen carrier gas.<h3>4. Thermo Fisher Scientific: Enhanced trace moisture analysis in organic solvents using GC with multi-channel VUV detection</h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_003954_gc_luma_detector_trace_1610_industrial_pharma_an003954_na_en_c29f4875a6.pdf">Full PDF for download</a></li></ul>Monitoring water content in organic solvents is essential across various industries, notably in pharmaceutical manufacturing, where excess moisture can compromise active ingredient stability. Traditionally, Karl Fischer titration has been the benchmark technique, offering broad quantification capability. However, KF is limited by side reactions, reagent sensitivity, and incompatibility with high-throughput workflows. It also relies on hazardous solvents and extensive manual steps.&nbsp;Gas chromatography provides an alternative means of quantifying water when paired with an appropriate detector. While FID and TCD have been used, they lack the selectivity and sensitivity required for trace moisture detection. Ionization-based detectors like PDD improve detection but suffer from dynamic range limitations.The <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=3&amp;search=LUMA%E2%84%A2+VUV+detector">LUMA™ VUV detector </a>(VUV Analytics, Inc.) overcomes these drawbacks by employing vacuum ultraviolet absorbance in the 118–240 nm range, where water exhibits strong and selective absorption. Unlike other GC detectors, LUMA combines universality, spectral selectivity, and ease of use in a single platform.&nbsp;This work illustrates a GC method using a LUMA Multi-Channel VUV Absorbance detector to analyze moisture in acetonitrile from 250 ppb up to percent levels. This approach has several advantages over traditional techniques like Karl Fischer titration, including superior sensitivity for the analysis of trace levels of water in acetonitrile as well as percent levels. The achievable limit of detection for water in acetonitrile is 250 ppb, with method linearity over 0.25–100 ppm producing R² ≥ 0.999.&nbsp;<h4>LUMA detector highlights&nbsp;</h4><ul><li>Detection range: 125–1,050 nm VUV-UV-VIS&nbsp;</li><li>Channel configuration: Up to 12 discrete absorbance bands simultaneously acquired&nbsp;</li><li>Sensitivity: Low-ppb to percent level in a single method&nbsp;</li><li>Installation: Compact, uses any carrier gas and no vacuum pumps&nbsp;</li><li>Software integration: Fully controlled via Thermo Scientific™ Chromeleon™ Chromatography Data System (CDS)&nbsp;</li></ul>These capabilities enable detection of water and organic solvents in a single injection—dramatically simplifying workflows in quality control laboratories.<h4>Experimental&nbsp;</h4>The LUMA detector can be easily installed on a <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/483">Thermo Scientific™ TRACE™ 1600 Series GC</a> and controlled in <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/76">Chromeleon CDS</a>, providing method settings, data acquisition, and reporting in a single software platform.GC-VUV separation using the LUMA Multi-Channel Vacuum Ultraviolet Absorbance detector was based on a previously described method by VUV Analytics.¹ Method conditions for this experiment are described in Table 1.A commercially available 100 ppm KF standard (water in xylene) was used to determine sensitivity, linearity, and repeatability. To minimize the impact of environmental moisture in this experiment, the same solution has been used to simulate different water levels through varying split ratios and injection volumes.&nbsp;Seven concentration levels (0.25–100 ppm) were created using adjusted split ratios as summarized in Table 2. Five replicate injections were made at each level.<h4>Key application benefits&nbsp;</h4><ul><li>Replaces Karl Fischer titration for routine moisture analysis&nbsp;</li><li>Simultaneous quantification of water and organic solvents&nbsp;</li><li>Ideal for pharmaceutical QA/QC and regulatory environments&nbsp;</li><li>Fast, automated workflows with no vacuum or specialty gases&nbsp;</li></ul>This workflow is aligned with recent trends toward hybrid analytical techniques that reduce resource consumption and speed up decision-making in GMP labs.&nbsp;<h4>Conclusion</h4>The LUMA multi-channel VUV detector offers a transformative approach to moisture analysis in volatile organic solvents. It provides both trace-level sensitivity and wide dynamic range— enabling labs to consolidate workflows, eliminate time-consuming titrations, and enhance data reliability.&nbsp;By expanding GC capability to encompass water detection, LUMA bridges a long-standing gap in chromatographic technology, delivering measurable gains in efficiency and analytical scope.&nbsp;<ul><li>The detector operates in the 125 nm to 1,050 nm region of the spectrum, where nearly all compounds absorb, making it a universal GC detector.&nbsp;</li><li>The detector associates high sensitivity to high selectivity thanks to the simultaneous acquisition of 12 channels with different spectral range in the VUV spectrum.&nbsp;</li><li>Working with up to 12 channels, the detector allows the determination of multiple analytes in a single injection. For example, water, solvents, and a range of impurities including potential genotoxic impurities (PGIs).&nbsp;</li><li>In addition to having high sensitivity and selectivity, the LUMA detector is easy to use; it is controlled by Chromeleon CDS, fitting well into existing laboratory workflows, and does not require a vacuum pump or separate special carrier gases.</li></ul>

News from LabRulezGCMS Library - Week 42, 2025

Our Library never stops expanding. What are the most recent contributions to LabRulezGCMS Library in the week of 20th October 2025? Check out new documents from the field of the gas phase, especially GC and GC/MS techniques!<blockquote>👉 <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library">SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT GCMS AND RELATED TECHNIQUES</a></blockquote><blockquote>👉 Need info about different analytical techniques? Peek into <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library">LabRulezLCMS</a> or <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library">LabRulezICPMS</a> libraries.</blockquote>This week we bring you applicaton notes by Agilent Technologies, EST Analytical, Shimadzu and Thermo Fisher Scientific!<h3>1. Agilent Technologies: FAMEs Analysis of Oils by GC-FID Coupled with Fully Automated Sample Preparation using a PAL3 Series 2 RTC</h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_fame_oil_gc_pal3_5994_8543en_agilent_418da94d17.pdf">Full PDF for download</a></li></ul>The analysis of fatty acid methyl esters (FAMEs) is a widely used technique for characterizing lipid profiles in various food products, including oils, meats, and seeds. Fats are composed of a complex mixture of saturated, monounsaturated, and polyunsaturated fatty acids, each with varying carbon chain lengths.2 This type of analysis is routinely performed in governmental, quality control (QC), and contract research laboratories worldwide. The resulting data often informs product labeling. Among the analytical techniques available, gas chromatography (GC) with flame ionization detection (GC-FID) is one of the most common methods for determining fatty acid composition in&nbsp;foods.&nbsp;This application note describes the use of automated sample preparation and analysis of FAMEs using the PAL3 Series&nbsp;2 RTC Autosampler system coupled with Agilent 8890 GC system equipped with an FID. The results shown here focus on two different methods of derivatization for FAMEs extraction: (1) base catalyzed reactions using potassium hydroxide (KOH) (part&nbsp;number M5795-14000) and (2) base plus acid catalyzed reactions using boron trifluoride (BF3 ) 1 (part number M5795-14001). For ease of use, both processes have been transcribed into dedicated sample preparation methods. These methods are part of the Agilent automated sample preparation workflow suite of solutions. These workflows improve process safety, optimizes throughput, and minimizes&nbsp;errors.<h4>Experimental&nbsp;</h4>The 37 component FAME mix standard was purchased from Sigma-Aldrich (part number CRM47885), and three consumer oil products were purchased from a local grocery store. The samples were prepared and injected into the GC using the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=PAL3">PAL3 Series 2-RTC system</a>. The analysis was performed using an <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=8890+GC">8890 GC</a> equipped with an <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=DB%E2%80%91FastFAME">Agilent DB‑FastFAME GC column</a>, 30&nbsp;m × 250 µm, 0.25&nbsp;µm, (part number G3903‑63011) and configured with an FID using Agilent&nbsp;<a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=OpenLab+CDS+v2.7">OpenLab CDS v2.7+</a>.<h4>Conclusion&nbsp;</h4>In summary, the current study demonstrated excellent reproducibility and accuracy using automated sample preparation and analysis of FAMEs. Two different sample preparation methods were demonstrated, both delivering comparable and reliable results. The base-catalyzed method enables rapid analysis but is not suitable for samples containing free fatty acids. In contrast, the acid-catalyzed method, while more extensive, is compatible with a broader range of lipid classes, including free fatty acids, phosphoglycerides, and triglycerides. The Agilent automated sample preparation workflow suite of solutions deliver a comprehensive package by combining preconfigured hardware, optimized analytical methods, and the necessary consumables to ensure efficient and reliable results.<h3>2. EST Analytical: Unregulated Contaminant Monitoring Rule 3 for USEPA Method 524.3 and 524.4</h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/Purge_and_Trap_Unregulated_Contaminant_Monitoring_Rule_3_for_USEPA_Method_524_3_and_524_4_b774e6ab4c.pdf">Full PDF for download</a></li></ul>The third Unregulated Contaminant Monitoring Rule (UCMR 3) was finalized in April of 2012. UCMR 3 requires public water systems to monitor for a specific list of 30 contaminants under three separate lists: list one, assessment monitoring, list two, screening survey, and list three, pre-screen testing. This application note will address the volatile organic compounds found in list one, assessment monitoring contaminants. USEPA Method 524.3 and 524.4 will be the methods evaluated for sampling and analysis.<h4>Discussion&nbsp;</h4>The amendments to the Safe Drinking Water Act (SDWA) require the EPA to list no more than 30 unregulated contaminants to be monitored by public water systems. Every five years, this list needs to be updated. List one contaminants include seven volatile organic compounds to be analyzed by USEPA Method 524.3. The detection limits for these compounds are much lower; therefore, Single Ion Monitoring (SIM) must be used for compound detection. USEPA Method 524.3 and 524.4 allow for modification of purge and trap parameters in order to take advantage of purge and trap improvements. Thus, method parameters can be modified in order to optimize purge and trap cycle times. Since the purge and trap parameters were established for these methods previously, refer to application note Drinking Water Analysis Conditions for USEPA Method 524.3 and the Newly Proposed Method 524.4, purge and trap method development was not required for this application. For this study, Helium and Nitrogen purge gases were compared utilizing the same purge volume then comparing experimental results for the linearity, precision, accuracy and overall compound response for the low level requirements set by UCMR 3.&nbsp;<h4>Experimental&nbsp;</h4>The <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/2160">EST Analytical Encon Evolution purge and trap concentrator</a> and <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/2159">Centurion WS autosampler </a>were interfaced to an <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=7890%2F5975">Agilent 7890/5975 GC/MS</a>. The purge and trap concentrator was configured with a Vocarb 3000 (K) analytical trap. A chiller unit capable of keeping the sample vials cooled below 10°C was installed on the Centurion WS autosampler. The experimental parameters are listed in Tables 1 and 2.<h4>Conclusion</h4>The Encon Evolution and Centurion WS in conjunction with the Agilent 7890/5975 GC/MS performed very well using both the Helium and Nitrogen purge gases and employing SIM for compound detection. The Nitrogen and the Helium purge gases met USEPA Method 524.3 curve linearity criteria and produced comparable results for precision and accuracy at the low and mid-levels of the calibration curve. Overall, the principal difference between the two purge gases was exhibited in the compound response. When examining the overall compound response factors over the curve range, it is evident that the analytes’ responses are slightly lower with the Nitrogen purge gas as opposed to the Helium purge gas.<h3>3. Shimadzu: Comparison of Metabolites in Rice from Different Production Areas Using GC-MS/MS</h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_01_01000_en_9c1d7cfe70.pdf">Full PDF for download</a></li></ul>Metabolomics is a research method for comprehensively analyzing metabolites contained in an organism. It is used for a wide variety of fields, such as medical science and food. Because food quality is affected by many components complexly, comprehensive analysis of metabolites can help improve food development and manufacturing processes. Rice contains metabolites, such as sugars, amino acids, and fatty acids. In recent years, development of more flavorful rice has been studied.&nbsp;This article describes simultaneous analysis of 502 metabolites and multivariate analysis of a variety of rice from different production areas. The <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=1&amp;search=GCMS-TQ8040+NX">GCMS-TQ8040 NX</a> with the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=1&amp;search=Smart+Metabolites+Database+ver.+2">Smart Metabolites Database Ver. 2</a> was used for measurement. <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=1&amp;search=LabSolutions+Insight">LabSolutions Insight </a>was used for data processing, and <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=1&amp;search=eMSTAT+Solution">eMSTAT Solution</a> was used for multivariate analysis. The process flow, from pretreatment to data analysis, is shown in Fig. 1.<h4>eMSTAT Solution&nbsp;</h4>eMSTAT Solution is statistical analysis software that enables multivariate and discriminant analysis of chromatogram data. For multivariate analysis, it can discriminate between samples, and it can search for the marker peaks that contribute to those differences. For discriminant analysis, it can create a discriminant model based on training data and use the model for discriminant analysis. Users can easily switch both modes with just a single click. Workflow of the data analysis is shown in Fig. 2.<h4>Conclusion&nbsp;</h4>Metabolites in same variety of rice from different production areas were analyzed, and the differences between samples were identified by multivariate analysis. Score plots were used to visualize differences between the samples, and loading plots were used to confirm the characteristic compounds. Smart Metabolites Database Ver. 2, LabSolutions Insight, and eMSTAT Solution make metabolites analysis, data processing, and multivariate analysis easy for beginner users.<h3>4. Thermo Fisher Scientific: Automated, multi-parameter gasoline characterization using GC-VUV and ASTM D8071</h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_003957_gc_vuv_trace_1610_vga_industrial_an003957_na_en_3c0a64e3b2.pdf">Full PDF for download</a></li></ul>Gasoline is a complex hydrocarbon blend whose composition directly impacts combustion behavior, emissions, and regulatory compliance. Accurately quantifying components such as aromatics, olefins, ethanol, and benzene is critical, but traditional ASTM methods require multiple techniques (FIA, GC-FID, GC-MS, etc.) to measure all relevant parameters. Table 1 summarizes several test methods and their respective scopes.&nbsp;ASTM D8071 introduces a consolidated method using GC-VUV, offering improved precision, spectral resolution, and reduced operational burden. This approach is now recognized as an EPA- and CARB-approved alternative to several legacy test methods, including ASTM D1319, D5599, D5769, and D3606.<h4>Experimental&nbsp;</h4>Gasoline samples were analyzed on the VUV Analyzer Platform for Fuels with no sample preparation required. The VUV Analyzer consists of the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/486">Thermo Scientific™ TRACE™ 1610 gas chromatograph</a> coupled to the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=3&amp;search=VGA-100">VGA-100™ spectrometer detector </a>(VUV Analytics, Inc.).&nbsp;Data are acquired and processed with the VUVision™ Software and VUV Analyze™ Software (VUV Analytics, Inc), respectively, specifically configured to run ASTM D8071.&nbsp;<h5>Workflow overview&nbsp;</h5>The VUV Analyzer Platform for Fuels performs gasoline PIONA class analysis using a streamlined five-step workflow:&nbsp;<ol><li>System validation – Verifies instrument performance using standard hydrocarbons.&nbsp;</li><li>Sample prep – No preparation required.&nbsp;</li><li>Data acquisition – Performed using VUVision Software.&nbsp;</li><li>Spectral matching – Automated deconvolution with VUV Analyze Software.&nbsp;</li><li>Quantitation – Volume % and mass % calculated with high accuracy using built-in response factors and density data.</li></ol><h4>Conclusion&nbsp;</h4>GC-VUV with ASTM D8071 enables complete hydrocarbon group and compound-level analysis of gasoline in a single method. Its ability to automate spectral deconvolution and report mass and volume percentages simplifies operations while meeting strict compliance standards. This solution not only enhances analytical accuracy and repeatability but also drastically reduces operating costs and lab complexity.&nbsp;<ul><li>Short analysis time with full gasoline class and compound profiling in 34 minutes&nbsp;</li><li>Faster throughput with full automation from injection to reporting&nbsp;</li><li>12× lower cost-per-analysis, due to reduced labor, no calibration standards, and consolidated workflow</li></ul>

News from LabRulezGCMS Library - Week 43, 2025

<h4>Abstract</h4>Strong or weak, light or dark, black or with cream; everyone who drinks coffee has a preference. Today, there are not only the choices of what you would like in your coffee, but also how you would like it brewed. Do you prefer the old fashioned percolator or the straight forward brewed coffee? Or do you like the new coffee by the cup makers or the instant coffees? There are so many options! This study will analyze four different instant coffee blends for some of their respective flavors using a purge and trap concentrator.<h4>Discussion</h4>Most of us who drink coffee know our preferences. We know which blend we like, what strength and definitely what we like in our coffee. However, most of us do not think about the flavors that go into our coffee that help us define our preferences. Coffee manufacturers, on the other hand, are working diligently to create a new blend or a more satisfying flavor that would make us want to choose their coffee over another maker.This study will look at four different blends of coffee and some of the compounds that contribute to the flavor of the blend. Using purge and trap sampling, the flavor compounds were purged out of the coffee and trapped onto an adsorbent trap. The analytes were then transferred to a Gas Chromatograph/Mass Spectrometer (GC/MS) for analysis. The study focused on six flavor compounds: the spicy smoky aroma of 2-methylfuran, the spicy caramel, almond odor of 5-methylfurfural, the buttery scent provided by the addition of 2,3-butanedione and 2,3-pentanedione, and the impact of the two and three methyl butanals giving the dark chocolate malty flavor to the coffee.<img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/EST_Analytical_Purge_and_Trap_Analysis_of_Coffee_Flavors_by_Purge_and_Trap_Sampling_ca25beef60_1_acf9fc0b4f.jpg" alt="EST Analytical: Encon Evolution Purge and Trap Concentrator and Centurion WS Autosampler" srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_EST_Analytical_Purge_and_Trap_Analysis_of_Coffee_Flavors_by_Purge_and_Trap_Sampling_ca25beef60_1_acf9fc0b4f.jpg 197w," sizes="100vw" width="668" height="531"><h4>Experimental</h4>The EST Analytical <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/2160">Encon Evolution Purge and Trap Concentrator</a> and <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/2159">Centurion WS Autosampler</a> were interfaced to a GC/MS. The Centurion WS was run in the soil mode and the purge and trap concentrator was configured with a Vocarb 3000 (K) analytical trap. The column selected for this study was an Rtx-1 60 m × 0.25 mm × 1 µm. Sampling method parameters and GC/MS parameters are listed below.<h5>Purge and Trap Parameters</h5><ul><li>Concentrator: EST Encon Evolution</li><li>Trap type: Vocarb 3000</li><li>Valve oven temperature: 150 °C</li><li>Transfer line temperature: 150 °C</li><li>Trap temperature: 35 °C</li><li>Moisture Reduction Trap (MoRT) temperature: 39 °C</li><li>Purge time: 11 min</li><li>Purge flow: 40 mL/min</li><li>Dry purge Temp.: Ambient</li><li>Dry Purge Flow: 50mL/min</li><li>Dry Purge Time: 1.0 min &nbsp;</li><li>Desorb pressure Control: ON</li><li>Desorb Pressure: 5psi</li><li>Desorb time: 0.5 min</li><li>Desorb preheat delay: 5 sec</li><li>Desorb temperature: 260 °C</li><li>MoRT bake temperature: 230 °C</li><li>Bake temperature: 260 °C</li><li>Sparge vessel bake temperature: 120 °C</li><li>Bake time: 8 min</li><li>Bake flow: 85 mL/min</li></ul><h5>Auto-Sampler (EST Centurion WS):</h5><ul><li>Sample type: Soil</li><li>Sample Fill Mode: loop</li><li>Sample Volume: 10mL</li><li>Sample Prime Time: 5 sec</li><li>Loop Equilibration Time: 10 sec</li><li>Sample Transfer Time: 15 sec</li><li>Sample Loop Rinse: Off</li><li>Sample Loop Sweep Time: 15 sec</li><li>Number of Sparge Rinses: 1</li><li>Rinse Volume: 5mL</li><li>Rinse Transfer Time: 20 sec</li><li>Rinse Drain Time: 20 sec</li><li>Number of Foam Rinse Cycles: 1</li><li>Water Heater Temp.: 85°C</li><li>Sample Preheat Temp.: 40°C</li><li>Soil Valve Temp.: 85°C</li><li>Soil Transfer Line Temp.: 150°C &nbsp;</li></ul><h5>GC/MS Parameters</h5><ul><li>System: <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=7890%2F5975">Agilent 7890/5975</a></li><li>Inlet: Split mode, 200 °C, 20:1 split ratio, 16.041 psi head pressure</li><li>Column: Rtx-1 60m x 0.25mm I.D. 1.0µm film thickness</li><li>Oven program: 35 °C (1 min) → ramp 4 °C/min → 230 °C, total run time of 49.75 min</li><li>Column flow rate: 1 mL/min helium</li><li>Total flow: 26.0 mL/min</li><li>Source temperature: 230 °C</li><li>Quadrupole temperature: 150 °C</li><li>Transfer line temperature: 180 °C</li><li>Scan range: m/z 35–265, 3.12 scans/sec</li><li>Solvent delay: 0.0 min</li></ul>The GC column was acquired from Restek while the instant coffees were purchased at a local retailer. The four roasts chosen for this study ranged from light to dark. One half of a gram of each coffee was dissolved in 40 mL of de-ionized water at room temperature. The vials were shaken in order to fully dissolve the coffee. Next, 5 mL of each coffee mixture were run in the soil mode using the Centurion WS autosampler and the Encon Evolution purge and trap concentrator. Each coffee was run in triplicate in order to verify the results. Figures 1 through 3 display a bar graph comparison of the flavors in each coffee blend. Chromatograms of the coffee blends are shown in Figures 4 through 7.<img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/EST_Analaytical_Figure_1_Buttery_Compound_Comparison_08f6fd5d05.jpg" alt="EST Analytical: Figure 1 Buttery Compound Comparison" srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_EST_Analaytical_Figure_1_Buttery_Compound_Comparison_08f6fd5d05.jpg 245w," sizes="100vw" width="905" height="544"><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/EST_Analaytical_Figure_2_Smoky_and_Spicy_Caramel_Compound_Comparison_6940d35e36.jpg" alt="EST Analytical: Figure 2 Smoky and Spicy Caramel Compound Comparison" srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_EST_Analaytical_Figure_2_Smoky_and_Spicy_Caramel_Compound_Comparison_6940d35e36.jpg 245w," sizes="100vw" width="905" height="545"><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/EST_Analaytical_Figure_3_Dark_Chocolate_Malty_Compound_Comparison_cbee579baf.jpg" alt="EST Analytical: Figure 3 Dark Chocolate - Malty Compound Comparison" srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_EST_Analaytical_Figure_3_Dark_Chocolate_Malty_Compound_Comparison_cbee579baf.jpg 245w," sizes="100vw" width="905" height="545"><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/EST_Analaytical_Figure_4_Light_Roast_Chromatogram_8380d110a6.jpg" alt="EST Analytical: Figure 4 Light Roast Chromatogram" srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_EST_Analaytical_Figure_4_Light_Roast_Chromatogram_8380d110a6.jpg 245w," sizes="100vw" width="953" height="375"><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/EST_Analaytical_Figure_5_Medium_Roast_Chromatogram_9a97a58a74.jpg" alt="EST Analytical: Figure 5 Medium Roast Chromatogram" srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_EST_Analaytical_Figure_5_Medium_Roast_Chromatogram_9a97a58a74.jpg 245w," sizes="100vw" width="886" height="401"><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/EST_Analaytical_Figure_6_Medium_Dark_Roast_Chromatogram_eb6a37cd16.jpg" alt="EST Analytical: Figure 6 Medium Dark Roast Chromatogram" srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_EST_Analaytical_Figure_6_Medium_Dark_Roast_Chromatogram_eb6a37cd16.jpg 245w," sizes="100vw" width="877" height="410"><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/EST_Analaytical_Figure_7_Dark_Roast_Chromatogram_79711f7858.jpg" alt="EST Analytical: Figure 7 Dark Roast Chromatogram" srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_EST_Analaytical_Figure_7_Dark_Roast_Chromatogram_79711f7858.jpg 245w," sizes="100vw" width="856" height="412"><h4>Conclusion</h4>The lightest roast had the most buttery and dark chocolate/malty flavors while the darkest roast had more of the smoky flavor. Surprisingly, the darkest roast and the medium roast had similar proportions of the flavor compounds with the exception of the smoky flavor. While the light roast had large amounts of the flavors tested for, the chromatography of the light roast was much simpler than that of the darker roasts. Overall, the Encon Evolution Purge and Trap Concentrator in conjunction with the Centurion WS Autosampler proved to be an excellent system for sampling coffee. The results were reproducible and provided a lot of information on the flavors of the respective coffees.

Analysis of Coffee Flavors by Purge and Trap Sampling

News from LabRulezGCMS Library - Week 44, 2025

Our Library never stops expanding. What are the most recent contributions to LabRulezGCMS Library in the week of 3rd November 2025? Check out new documents from the field of the gas phase, especially GC and GC/MS techniques!<blockquote>👉 <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library">SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT GCMS AND RELATED TECHNIQUES</a></blockquote><blockquote>👉 Need info about different analytical techniques? Peek into <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library">LabRulezLCMS</a> or <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library">LabRulezICPMS</a> libraries.</blockquote>This week we bring you applicaton notes by Agilent Technologies, EST Analytical and Thermo Fisher Scientific and poster by Shimadzu!<h3>1. Agilent Technologies: Estimation of Methyl Bromide Residues in Food</h3>Using the Agilent 8890 GC and Agilent 7010 triple quadrupole GC/MS system with Agilent 8697 headspace sampler<ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_methyl_bromide_food_8890_gc_7010_tq_8697_hs_5994_8499en_agilent_35c0751a37.pdf">Full PDF for download</a></li></ul>Bromomethane (methyl bromide) is a halogenated hydrocarbon with a boiling point of 3.6 °C. It is widely used as a fumigant due to its strong fumigation and penetration effects, effectively controlling pests.1 However, methyl bromide is harmful to the ozone layer, causes environmental pollution, and is harmful to humans.2 By 2015, most countries phased out its production and application, except for essential uses such as port quarantine. China stopped agricultural use of methyl bromide by the end of 2018.2 Despite its high volatility, residues of methyl bromide can persist in foods such as nuts and seeds. Therefore, quantitative methods for determining these residues are important. Gas chromatography (GC) is commonly used for analysis, either directly with headspace sampling, or with sample pretreatment methods including solvent extraction and solid phase microextraction. Various detectors are used with GC, such as the flame ionization detector, electron capture detector, and electron ionization. Detection can also be performed by mass spectrometer, using an electron ionization (EI) source. The maximum residue limit for methyl bromide in the EU is 10&nbsp;ng/g, according to EU Regulation number 396/2005.&nbsp;In this application note, an <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=1-10&amp;search=8697+headspace+">Agilent 8697 headspace sampler</a> was used for sample introduction to an <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=1-10&amp;search=8890">Agilent 8890 GC system</a> coupled with an <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=7010">Agilent 7010 triple quadrupole GC/MS</a> for quantification of methyl bromide residues.<h4>Results and discussion&nbsp;</h4><h5>Calibration&nbsp;</h5>Figures 1 through 3 show the linearity of the methyl bromide calibration curve in rice, cumin powder, and red chili powder, respectively. The R2 obtained was above 0.998.&nbsp;<h5>Repeatability&nbsp;</h5>The repeatability of this method was demonstrated by injecting six replicates of rice, cumin, and red chili powder spiked with 10 ng/g of methyl bromide. The area %RSD and retention time %RSD results are shown in Table 3.&nbsp;<h5>Recovery&nbsp;</h5>Methyl bromide was spiked in samples of rice, cumin, and red chili powder at concentration levels of 10 ng/g. Acceptable recoveries were obtained by quantification through prespike matrix-based calibration. Results are highlighted in Table 4.<h4>Conclusion&nbsp;</h4>An accurate and rugged method was developed which meets the requirements of the EURL for the maximum residue limit of methyl bromide in foodstuffs. This ranges from 10 to 100 ng/g, depending on the commodity (Reg. (EC) number 396/2005) for the analysis of pesticides in rice, cumin powder, and red chili powder. The LOQ of the method was demonstrated at 5 ng/g for all tested matrices. Repeatable results were found for six successive replicates of matrix‑based standards at 10 ng/g concentration levels. Sufficient recoveries were obtained in all tested matrices at 10 ng/g spiked concentration levels. Thus, this study demonstrates the applicability of this method for routine analysis of food samples for methyl bromide at trace levels.<h3>2. EST Analytical: Effect of Split Ratio on USEPA Method 8260 Compounds</h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/Purge_and_Trap_Effect_Split_Ratio_on_USEPA_8260_Compounds_2b7339c7c7.pdf">Full PDF for download</a></li></ul>Injection size on a GC column is dictated by the diameter of the GC column. Packed columns are usually shorter in length and larger in diameter and are usually filled with a packing coated with stationary phase. Due to their large diameter, packed columns can handle much larger injections. However, since packed columns are shorter in length, compound resolution is more difficult. Capillary columns, on the other hand, are much longer with much smaller diameters. A capillary column has a stationary phase that is coated onto the column wall which in turn makes the diameter even smaller. Overloading is a common problem with capillary columns, thus smaller injections and higher dilutions are required when using a capillary column.&nbsp;The benefit of a capillary column is that it has substantially more theoretical plates than a packed column. Increasing the number of theoretical plates enhances column efficiency because peaks are narrowed and peak resolution is improved. The disadvantage of the capillary column is column overloading. This is where a split injection is greatly beneficial. A split injection can limit sample overload while taking advantage of the efficiency of the capillary column.&nbsp;<h4>Discussion:&nbsp;</h4>Purge and trap sampling is the method used for purging volatile compounds out of a water matrix for USEPA Method 8260. Due to the large number of analytes and the lower detection limits required in this method, a capillary column is needed for detection and separation. Split injections provide a method to control moisture from the purge and trap sampling while preventing column overloading with the capillary column. However, due to the detection limits required of the method, if the split injection is too large, the detection limits of the method may not be met. On the other hand, if the split injection is too small, there can be moisture problems with the mass spectrometer. This application will provide a comparison of several different split rates and their effect on compound detection for USEPA Method 8260.<h4>Experimental:&nbsp;</h4>The sampling system used for this study was the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/2160">EST Analytical Evolution concentrator</a> and the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/2159">Centurion WS autosampler</a>. The concentrator was affixed with a Vocarb 3000 trap and connected to an <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=1-10&amp;search=7890A">Agilent 7890A GC</a> and <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=1-10&amp;search=5975C">5975C </a>inert XL MS. The GC was configured with a Restek Rxi-624 Sil MS 30m x 0.25mm x 1.4µm column. Three different split ratios were used for this study. Refer to Table 1 for the sampling method parameters and Table 2 for GC/MS parameters.<h4>Conclusions:&nbsp;</h4>As USEPA Methods require lower and lower detection limits, split ratios will play a large factor in reaching these new requirements. This study demonstrated that all three split ratios met USEPA Method 8260 requirements for linearity, compound response and method detection limits. However, there was a remarkable difference in compound detection limits as the split ratio was increased. The 40 to 1 split rate had much lower detection limits due to an increase in compound response. The Encon Evolution purge and trap concentrator has a unique feature for moisture control using an eight port valve to avoid desorbing through the moisture trap. This feature enables better moisture control when using a lower split rate, thus using a larger split rate to control moisture is unnecessary.<h3>3. Shimadzu / AOAC: Simultaneous analysis of residual contaminants in drinking water using Programmed Temperature Vaporization (PTV) for Large Volume Injection (LVI) and GC-MS/MS</h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/aoac_2025_w016_04bda0b617.pdf">Full PDF for download</a></li></ul>This study aimed to develop a single analytical method for the simultaneous analysis of over 60 residual contaminants, including Poly-Aromatic Hydrocarbons (PAH), Poly-Chlorinated Biphenyls (PCB), and pesticides, in drinking water. Traditionally, multiple methods are being employed for analyzing these contaminants. Most common ones include, extraction using solvents in large separating funnel or SPE cartridge followed by volume concentration by evaporation. These methods require huge sample and solvent quantities. Due to these factors like large sample size handling, concentration steps etc., method may show poor reproducibility.&nbsp;By utilizing Programmed Temperature Vaporization (PTV) for Large Volume Injection (LVI), the method significantly reduces the initial sample amount required for preparation, pre-treatment steps, and solvent consumption compared to conventional approaches, while eliminating the need for final sample concentration. The optimized procedure achieved limits of quantification (LOQs) as low as 0.005 ppb and 0.05 ppb, demonstrating high sensitivity without compromising efficiency. Validation parameters like specificity, linearity, recovery and precision were studied as per SANTE guidelines[1] . For linearity and recovery study, matrix match calibration was used.<h4>Materials and methods&nbsp;</h4>For this study, reference standard mixtures of over 60 contaminants regulated in drinking water were procured from Restek® Corporation. It included PAH, PCB and GC amenable pesticides. Drinking water sample was extracted and used to prepare matrix-matched calibration standards and spiked samples. This method was validated for criteria mentioned in SANTE Guidelines. <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=1&amp;search=GCMS-TQ8040+NX">GCMS-TQ8040 NX</a> (Figure 2), manufactured by Shimadzu Corporation Japan, was used to quantify residual contaminants in drinking water sample.<h4>Conclusion</h4><ul><li>This study shows that the extraction of reduced sample quantity combined with LVI of 50 μL on GC-MS/MS system is a reliable and efficient tool to simultaneously quantify residual contaminants like PAH, PCB and pesticides in drinking water sample.</li><li>Also, highly sensitive Shimadzu GC-MS/MS allows trace level detection even without the need of evaporating &amp; concentrating the sample. This helps in ruggedness resulting in reproducible detection of analytes.</li><li>The combination of sensitive instrument and reproducible extraction method enables its use in testing laboratories for residual contaminants analysis in drinking water.</li></ul><h3>4. Thermo Fisher Scientific: Automated liquid-liquid extraction workflow for direct ultra-trace analysis of pesticides and PAHs in water matrices using GC-MS/MS</h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_003943_gc_autosampler_triplus_rsh_smart_environmental_an003943_na_en_b9980f4e3e.pdf">Full PDF for download</a></li></ul>Ensuring high standards of water quality is a fundamental priority within the European Union. This is highlighted through stringent EU regulations, such as the Water Framework Directive and the Drinking Water Directive,1 where protection of the environment and safeguarding public health are of utmost importance. As such, regular monitoring of both surface and drinking water for hazardous semi-volatile organic compounds, such as polyaromatic hydrocarbons (PAHs) and pesticides, is needed.1,2&nbsp;To meet regulatory compliance, laboratories are required to reach ultra-trace levels (i.e., parts per-trillion (ng/L)), while maintaining analytical method performance criteria outlined under EU Directive 2020/2184.3 To reach required concentration limits, laboratories typically need to extract large sample volumes using solvent (i.e., liquid-liquid) or sorbent-based (i.e., solid-phase) extraction techniques with additional preconcentration.Such techniques involve manual operations, which are costly in terms of consumables and time. However, automated sample preparation and extraction can reduce such costs while helping to eliminate systematic errors to improve data quality and lab efficiency.&nbsp;The aim of this work was to evaluate the sensitivity, precision, and robustness of the TriPlus RSH SMART autosampler in performing automated liquid-liquid extraction and on-line analysis of polyaromatic hydrocarbons (PAHs) and pesticides in drinking and surface water using triple quadrupole GC-MS/MS. This study will demonstrate that the developed automated workflow is compliant with EU regulation criteria and greatly increases laboratory productivity by reducing laboratory costs and time.<h4>Experimental</h4><h5>Instrument and method setup&nbsp;</h5>A <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/486">Thermo Scientific™ TRACE™ 1610 GC </a>equipped with a <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/1744">Thermo Scientific™ TraceGOLD™ TG5-SilMS</a> (30 m × 0.25 mm I.D. × 0.25 µm film) capillary column with a 5 m integrated SafeGuard retention gap (P/N 26096-1425) was used to perform the chromatographic separation. The <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/422">TriPlus RSH SMART autosampler</a> was configured to perform automated sample preparation, liquid-liquid extraction, and on-line injection for GC-MS/MS analysis. The automated workflow was designed using the Thermo Scientific™ TriPlus™ RSH Sampling Workflow Editor Software (P/N 1R77010-1200) and imported into the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/76">Thermo Scientific™ Chromeleon™ 7.3.2 Chromatography Data System (CDS) software</a>. This integration allows sample preparation, acquisition, and data processing to be carried out within a single software. The automated workflow involved the following steps: internal standard addition, extraction solvent addition (pentane) and vortexing for extraction, addition of solvent for emulsion removal (isopropyl alcohol), addition of syringe standard prior to analysis, and large volume injection into the GC-MS. Parameter settings for the automated workflow are outlined in Table 1 with a visual overview provided in Figure 1. A list of accessories needed to configure the TriPlus RSH SMART autosampler is provided in the appendix (Table A2).&nbsp;After sample extraction was completed, a 30 μL aliquot of the pentane layer was directly injected into a programmable temperature vaporization (PTV) inlet. Injection and oven program conditions can be found described in Tables 1 and 2. Data acquisition was carried out using selected reaction monitoring (SRM) with a <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/485">Thermo Scientific™ TSQ™ 9610 triple quadrupole GC-MS</a> equipped with an Advanced Electron Ionization (AEI) source. Method parameters for data acquisition are summarized in Table 2 with optimized SRM transitions outlined in the appendix (Table A3).<h4>Conclusions&nbsp;</h4>Maintaining water quality is of both human and environmental health importance. However, due to the physical chemical properties of various organic substances, analytical methods require ultra-trace sensitivity and accuracy to quantify hazardous risks within both drinking and environmental surface waters. The results presented demonstrate that the developed automated workflow for online liquid-liquid extraction and analysis of water samples can meet these requirements:&nbsp;<ul><li>Ultra-trace sensitivity combining large volume injection with highly sensitive triple quadrupole GC-MS/MS, with over 70% of targeted analytes having limits of quantification below 2 ng/L&nbsp;</li><li>Compliant extraction recovery at part per trillion concentrations&nbsp;</li><li>Robust method precision over extended analysis time&nbsp;</li><li>Improved laboratory efficiency and productivity while reducing environmental impact with limited solvent consumption&nbsp;</li><li>Workflow customization capability through the Sampling Workflow Editor software</li></ul>

News from LabRulezGCMS Library - Week 45, 2025

Analysis of field samples in environmental laboratories can sometimes be complicated by how contaminated or “hot” the sample is. Many times “hot” samples have to be diluted in order to verify the level of contamination in the sample. The process of diluting samples is a time consuming process that can sometimes lead to human error when calculations are incorrect. A further problem is the loss of volatile organic compounds as the sample vial needs to be opened in order to perform the dilution.&nbsp;This poster will examine the benefits of automated dilutions. Since the syringe option of this system has the unique ability to dilute samples from two times to 400 times the original concentration, this study will examine the precision and accuracy for an array of dilutions in this comprehensive range. The dilution data will be compared to a manually prepared 50ppb calibration standard in order to determine the accuracy of the results. The precision will be established by examining four sequential dilutions and the percent relative standard deviation of the compounds’ respective area counts. Furthermore, in order to demonstrate the linearity of the dilutions, a calibration curve will be presented using the automated dilution option to prepare 200ppb standards for a calibration range of 0.5ppb (400x) to 200ppb (1x).<h4>Discussion&nbsp;</h4>Environmental laboratories often have to dilute field samples due to the analytes of interest having concentrations over the highest calibration level of the curve. In order to dilute these samples, the vial has to be opened and a portion of the sample has to be diluted manually and re-analyzed. Opening the vial can compromise the integrity of the sample as volatiles are lost when the seal of the vial is broken.&nbsp;EST Analytical has developed a syringe feature for the Centurion Autosampler that can dilute samples up to 400 times the original concentration. This feature is fully programmable and the sample vial does not have to be compromised in order to dilute the sample because the dilution process is automated. The sealed vial can be placed in the sample tray while the Centurion does all of the work.&nbsp;<h4>Experimental&nbsp;</h4>The <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/2159">Centurion WS autosampler</a> was configured with an <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/2160">Encon Evolution concentrator</a>. A Vocarb 3000 (K) trap was installed in the Evolution. Finally, the sampling system was connected to a GC/MS for sample analysis. The GC column employed for this study was an Rxi-624Sil MS 30m x 0.25mm x 1.4µm. Dilution Factors, Purge and Trap, and GC/MS parameters are listed below.<h5>Standard Concentration &amp; Dilution Factors</h5><ul><li>100ppb: 2x</li><li>250ppb: 5x</li><li>500ppb: 10x</li><li>2.5ppm: 50x</li><li>5ppm: 100x</li><li>10ppm: 200x</li><li>20ppm: 400x</li></ul><h5>Purge and Trap Parameters</h5><ul><li>Concentrator: EST Encon Evolution</li><li>Trap type: Vocarb 3000</li><li>Valve oven temperature: 150 °C</li><li>Transfer line temperature: 150 °C</li><li>Trap temperature: 35 °C</li><li>Moisture Reduction Trap (MoRT) temperature: 39 °C</li><li>Purge time: 11 min</li><li>Purge flow: 40 mL/min</li><li>Dry purge Temp.: Ambient</li><li>Dry Purge Flow: 40mL/min</li><li>Dry Purge Time: 1.0 min &nbsp;</li><li>Desorb pressure Control: ON</li><li>Desorb Pressure: 5psi</li><li>Desorb time: 0.5 min</li><li>Desorb preheat delay: 5 sec</li><li>Desorb temperature: 260 °C</li><li>MoRT bake temperature: 230 °C</li><li>Bake temperature: 265 °C</li><li>Sparge vessel bake temperature: 120 °C</li><li>Bake time: 8 min</li><li>Bake flow: 40 mL/min</li></ul><h5>GC/MS Parameters</h5><ul><li>System: <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=7890%2F5975">Agilent 7890/5975</a></li><li>Inlet: Split mode, 200 °C, 40:1 split ratio, 12.153 psi head pressure</li><li>Column: Rxi-624Sil MS 30m x 0.25mm I.D. 1.4µm film thickness</li><li>Oven program: 45 °C (1 min) → ramp 18 °C/min → 220 °C, hold for 0.3 min</li><li>Column flow rate: 1 mL/min helium</li><li>Total flow: 44.0 mL/min</li><li>Source temperature: 230 °C</li><li>Quadrupole temperature: 150 °C</li><li>Transfer line temperature: 180 °C</li><li>Scan range: m/z 35–265, 3.12 scans/sec</li><li>Solvent delay: 0.7 min</li></ul>A 9 point calibration curve was manually prepared and run from 0.5 to 200ppb with standards ordered from Restek. After a linear calibration curve was established, a 50ppb calibration standard was run to establish instrument response for the compounds being analyzed. Next, a series of dilutions were run and compared with the initial 50ppb calibration standard. Each dilution factor was run four times with blanks in between. The final concentration of each dilution was 50ppb. The precision and accuracy of the dilutions are listed in Tables 4 and 5 and Figures 1 and 2 display the chromatograms of two of the dilutions.<img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/EST_Analytical_Figure_1_Overlay_of_50ppb_1_X_and_2500ppb_50x_Standards_29d90b4107.jpg" alt="EST Analytical: Figure 1 - Overlay of 50ppb (1X) and 2500ppb (50x) Standards" srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_EST_Analytical_Figure_1_Overlay_of_50ppb_1_X_and_2500ppb_50x_Standards_29d90b4107.jpg 245w," sizes="100vw" width="1023" height="383"><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/EST_Analytical_Figure_2_Overlay_of_50ppb_1_X_and_10000ppb_200x_Standards_7f939589b9.jpg" alt="EST Analytical: Figure 2 - Overlay of 50ppb (1X) and 10000ppb (200x) Standards" srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_EST_Analytical_Figure_2_Overlay_of_50ppb_1_X_and_10000ppb_200x_Standards_7f939589b9.jpg 245w," sizes="100vw" width="1073" height="383"><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/EST_Analytical_Table_4_Experimental_Results_2x_5x_10x_and_50x_dilutions_d81be1942f.jpg" alt="EST Analytical: Table 4 - Experimental Results (2x, 5x, 10x, and 50x dilutions)" srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_EST_Analytical_Table_4_Experimental_Results_2x_5x_10x_and_50x_dilutions_d81be1942f.jpg 150w," sizes="100vw" width="1173" height="1220"><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/EST_Analytical_Table_5_Experimental_Results_100x_200x_and_400x_dilutions_f29762c72e.jpg" alt="EST Analytical: Table 5 - Experimental Results (100x, 200x and 400x dilutions)" srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_EST_Analytical_Table_5_Experimental_Results_100x_200x_and_400x_dilutions_f29762c72e.jpg 124w," sizes="100vw" width="972" height="1226">Finally, a nine point calibration curve was run by setting up the system to do the dilutions. The curve was run using nine 40ml vials filled to volume with a 200ppb calibration standard and doing serial dilutions on the standards. For example, the 200ppb was diluted 400x for the 0.5ppb standard, 200x for the 1.0ppb standard, etc. See Table 6 for the curve dilutions and Table 7 for the curve linearity and compound responses.<img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/EST_Analytical_Table_6_Syringe_Curve_Dilutions_4237e1d568.jpg" alt="EST Analytical: Table 6 Syringe Curve Dilutions" srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_EST_Analytical_Table_6_Syringe_Curve_Dilutions_4237e1d568.jpg 245w," sizes="100vw" width="785" height="381"><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/EST_Analytical_Table_7_Automated_Dilution_Curve_Results_356126f34f.jpg" alt="EST Analytical: Table 7 Automated Dilution Curve Results" srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_EST_Analytical_Table_7_Automated_Dilution_Curve_Results_356126f34f.jpg 138w," sizes="100vw" width="927" height="1050"><h4>Conclusions&nbsp;</h4>The Centurion WS with the syringe option displayed remarkable precision and accuracy from as low as the 2x dilution to as high as 400x dilution. On the whole, the average precision of the instrument was less than 5%RSD while the overall accuracy was 90% to 110%. The system also is capable of curve automation with the average %RSD of below 10% for a 9 point curve from 0.5ppb to 200ppb. The automated dilution feature of the Centurion WS with the syringe option would enable laboratories to run samples more efficiently and the since the samples would not need to be compromised in order to perform dilutions, the accuracy of the experimental results would improve.

Automated Dilutions Using the Centurion Autosampler

Our Library never stops expanding. What are the most recent contributions to LabRulezGCMS Library in the week of 10th November 2025? Check out new documents from the field of the gas phase, especially GC and GC/MS techniques!<blockquote>👉 <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library">SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT GCMS AND RELATED TECHNIQUES</a></blockquote><blockquote>👉 Need info about different analytical techniques? Peek into <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library">LabRulezLCMS</a> or <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library">LabRulezICPMS</a> libraries.</blockquote>This week we bring you applicaton notes by Agilent Technologies, EST Analytical and Shimadzu!<h3>1. Agilent Technologies: Improved Thermal Stability Leads to Retention Time Stability and Data Accuracy for the Analysis of Pesticides</h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_pesticide_gc_ms_5994_8447en_agilent_773f1f135b.pdf">Full PDF for download</a></li></ul>The analysis of trace-level pesticides is required by many governmental regulatory authorities at varying concentrations and can include hundreds of target analytes. As many of the matrices tested are complex and the analytes active, a robust and inert gas chromatography method is required.1 Heavy matrices can be difficult for analytical gas chromatography columns, and higher temperatures may be required to elute the matrix off of the column. To avoid damage from high temperatures and heavy matrix, a thermally stable and ultra inert analytical column phase is needed to successfully perform this analysis. The Agilent J&amp;W 5Q series of gas chromatography columns provide the most thermally stable column available and offer inertness for difficult analytes.2 The increased thermal stability not only dramatically reduces column bleed but also allows for less spectral interference at higher temperatures, leading to less need for background subtraction when searching analyte spectra against commercially available libraries.&nbsp;While column bleed is a normal phenomenon, the increase of the baseline due to column bleed is an indication of the column phase breaking down and leading to retention time shifts. Retention time shifting can be especially difficult with the analysis of pesticides, since sensitive detectors such as mass spectrometers and triple quadrupole systems collected in selected ion mode (SIM) or multiple reaction monitoring (MRM) mode are required to achieve lower limits of detection. In both SIM and MRM collection methods, time segment windows are stated for analytes of interest, and if a retention time shifts earlier, it can move out of the collection window and require time to update the analytical collection method. By using a GC column with increased thermal stability, such as the Agilent J&amp;W DB-5Q or the Agilent J&amp;W HP-5Q, the column will be more robust to thermal and matrix damage. These columns will also maintain consistent retention times over long periods of analytical stress.&nbsp;Retention time locking is a useful tool in the analysis of pesticides, as it can adjust column flow or pressure to normalize retention times, so that the retention times of the analytes are the same from system to system or column to column.3,4 When columns with identical selectivity are interchanged, after a single injection of a test mix, the analysis can be relocked and the column flow adjusted, based on the initial calibration, to be identical as in the original method. This eliminates the need to constantly update retention times in analytical methods for SIM or MRM windows or data processing methods when replacing analytical columns.&nbsp;When analyzing pesticides in heavy matrix, a guard column can serve two additional benefits. The guard column can help protect the analytical column from heavy matrix damage and can improve solvent and sample focusing. It is recommended to use nonpolar solvents when working with nonpolar column phases, such as the DB-5Q and HP-5Q columns. Recently it has become more common to prepare heavy matrices for pesticide analysis using QuEChERs-type preparations, with a final solvent of acetonitrile. Solvent-column phase polarity mismatch can lead to improper solvent focusing and wettability leading to improper peak shape, especially when working with columns that have low free silanol content on the deactivated surface of the fused silica. Use of a guard column can help to refocus the solvent and analytes to maintain proper peak shape.5&nbsp;The Agilent 7010D GC/TQ uses the new Agilent High Efficiency Source (HES) 2.0 equipped with a novel dipolar RF lens that redirects carrier gas and low mass ions by &gt;&nbsp;95%, helping to reduce noise and extend instrument robustness while maintaining sensitivity.6 When using DB-5Q and HP‑5Q columns in conjunction with the HES 2.0, it is possible to increase the overall robustness of the workflow for the analysis of pesticides over a wide dynamic range of analyte&nbsp;concentrations.&nbsp;<h4>Experimental&nbsp;</h4>An <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=8890">Agilent 8890 GC</a> coupled with an <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=5977B">Agilent 5977B GC/MSD</a> with an Inert Extractor Source was used for acquisition of data and <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=MassHunter+10.0+Qualitative+Analysis">MassHunter 10.0 Qualitative Analysis software</a> was used for data analysis. NIST20 library was used to confirm peak identification. A retention gap of one meter was used as a guard column to help protect the analytical column from heavy matrix and to aid in solvent focusing.<h4>Results and discussion&nbsp;</h4>The analysis of pesticides requires retention time stability as well as consistency from analytical column to analytical column. To compare the analytical performance of an Agilent J&amp;W DB-5Q to an Agilent J&amp;W DB-5ms UI GC column for the analysis of pesticides, a standard was first analyzed on a DB-5ms UI and the retention time locked for chlorpyrifosmethyl. The DB-5ms UI column was then replaced with a DB-5Q, and once the column was conditioned, the representative pesticide mix was again analyzed and relocked to the appropriate retention time for chlorpyrifos-methyl and analyzed again. Figure 1 demonstrates the identical selectivity of the DB-5ms UI to the DB-5Q phases and the ability to relock an existing analytical method when upgrading columns and compatibility with existing retention time locking libraries.&nbsp;Additionally, when comparing the baseline of the DB-5Q to the DB-5ms UI column at the upper temperature limit of the chromatographic method, the increased thermal stability of the DB-5Q allows for a significant decrease in column bleed at upper temperature limits (Figure 1).<h4>Conclusion&nbsp;</h4>This application note demonstrated that the Agilent J&amp;W DB-5Q column has identical selectivity to the Agilent J&amp;W DB-5ms UI column, allowing for seamless adoption and use with existing retention time locking methods. The robust DB-5Q column phase maintained retention time stability even when analyzing heavy matrices and temperature cycling. The increased thermal stability not only decreased the baseline at higher temperatures but also allowed for less spectral interference and high library match factor scores. The analytical performance of the Agilent J&amp;W DB-5Q column coupled with the Agilent 7010D with the HES 2.0 ion source allows for optimal sensitivity and wide dynamic range of pesticide compounds.<h3>2. EST Analytical: Automated Sampling of Methanol Extractions</h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/Purge_and_Trap_Automated_Sampling_of_Methanol_Extractions_f521577cc4.pdf">Full PDF for download</a></li></ul>Environmental labs are required to perform methanol extractions on highly contaminated solid waste samples. Additionally, these extractions are used for difficult matrices, for example oily waste samples, that are also soluble in methanol. Due to the variety of matrices that can be extracted with methanol there are assorted hurdles to cross in order to automate the sampling process. One of these obstacles is how the matrix can absorb the extraction solvent. For example, many soil samples require more methanol; due to the soil expanding with the solvent addition. Adding more methanol aids in rectifying this issue however, when automating sampling, the added methanol coupled with the soil expansion needs to be accommodated. For this reason, EST Analytical created software for the Centurion WS that allows the user to program the needle depth to different distances. In doing this, laboratories are able to sample soils at higher depths in order to adjust for sample absorption and at lower depths for samples that do not require the added solvent. In order to test volatile compounds in methanol extractions, a portion of the extract needs to be sampled from the vial, diluted, and purged on a purge and trap concentrator. This examination will look at the automated sampling of three different soil matrices.&nbsp;<h4>Experimental:&nbsp;</h4>The <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/2159">Centurion WS autosampler</a> with the syringe option and the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/2160">Evolution purge and trap concentrator</a> were set up to run methanol extractions. Since this is a volatile analysis, a Vocarb 3000 (K) trap was used for the analytical trap. The sampling system was configured to an <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=1-10&amp;search=7890A">Agilent 7890A Gas Chromatograph (GC)</a> and an <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=1-10&amp;search=5975C">Agilent 5975C inert XL Mass Spectrometer (MS)</a>. The column selected for this analysis was a Restek Rxi®-624 Sil MS, with dimensions of 30m x 0.25mm I.D. x 1.4µm film thickness. Experimental parameters used for this analysis are listed in Tables 1 and 2.<h4>Conclusions:&nbsp;</h4>The system produced excellent results. The curve and the compound response factors met all of the method requirements. The overall precision was less than 5% RSD while the system showed an average recovery of 94%. When examining the expected analyte concentration to the extracted sand results, it was found that the average recovery was approximately 102%. Thus, the automated extraction performed extremely well. When comparing the three different matrices it was found that they all displayed similar recoveries, however the sand matrix did perform the best of the three as expected since sand tends not to absorb analytes as readily as other matrices. Finally, the ability to control the needle depth on extraction samples was a great benefit for the different matrices as the system exhibited no issues with needle clogging due to the higher needle depth when performing the potting soil extractions. As demonstrated from this study, the Centurion WS automated extraction capability would be an asset to any lab performing extractions.<h3>3. Shimadzu: Fatty Acid Analysis of Edible Oils by GC</h3>Comparing Helium and Hydrogen as Carrier GasesComparing Analysis by GC with a Simple Screening Analysis by LC-MS<ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_01_00852_en_e928ab40ea.pdf">Full PDF for download</a></li></ul>There are a variety of edible oils that are sold commercially for a range of uses. They are almost entirely composed of compounds called triacylglycerols (neutral lipids), which consist of three fatty acids bound to a glycerol molecule. Because fatty acids affect the functional characteristics of food, determining the fatty acid composition of food is an important area of analysis. In this Application News, the Brevis GC-2050 (GC-FID) is used to determine the fatty acid composition of commercially available edible oils, and the use of hydrogen as a carrier gas is examined and compared with helium. This Application News also analyzes the same edible oils analyzed by LC-MS in a previous Application News1) and comparesthe results.<h4>Equipment&nbsp;</h4>GC-FID analysis was performed using the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=1&amp;search=Brevis+GC-2050">Brevis GC-2050</a> gas chromatograph (Fig.1) , which is designed to be highly compact, with an installation footprint 35 % smaller than the previous model. The Brevis GC-2050 is also equipped with a carrier gas saving mode that reduces carrier gas consumption. The carrier gas saving mode reduced the use of helium carrier gas by around 89 % and hydrogen carrier gas by around 79 % in the analyses described in this article. Hydrogen carrier gas also reduced analysis times by around 25 %.<h4>Results from Real-World Sample Analysis&nbsp;</h4>Edible oils were derivatized and analyzed using both helium and hydrogen carrier gases. Peaks that could not be identified with the calibration standard (37 FAME mixture) were analyzed by GC-MS to determine their carbon number and degree of unsaturation. (Labeled as isomer.) Fig. 4 shows the chromatograms (partial) obtained from analyzing linseed oil with helium and hydrogen carrier gases. Similar separation was achieved with both gases.<h4>Comparing GC-FID and FIA-MS&nbsp;</h4>Tables 5 and 6 compare the results of analyzing eight vegetable oils for fatty acids by FIA-MS (screening analysis) and GC-FID (a helium carrier). The results reveal characteristic features of the vegetable oils, such as the most abundant fatty acids, and that coconut oil contains fatty acids with relatively low carbon numbers. More information about the screening analysis performed with a single quadrupole mass spectrometer can be found in Shimadzu Application News 01-00674-EN. 1)<h4>Conclusion&nbsp;</h4>In this Application News, the Brevis GC-2050 was used to determine the fatty acid composition of edible oils. Fatty acid analysis is typically performed using helium as the carrier gas, but in this study, hydrogen was used. This reduced analysis times while producing results that compared favorably with helium. Given the current supply issues associated with helium, hydrogen should be considered as an alternative to helium.&nbsp;The results also show that fatty acid compositions determined by FIA-MS correlate well with results obtained by GC-FID. And because the sample pretreatment only requires sample dilution, analysis by FIA-MS is rapid, taking just 1 minute. Therefore, FIAMS seems particularly well-suited to the screening of large numbers of samples or when there is an urgent need to verify quality or safety

News from LabRulezGCMS Library - Week 46, 2025

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