Our Library never stops expanding. What are the most recent contributions to LabRulezGCMS Library in the week of 17th 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: Accurate Identification and Quantification of Pesticide Residues in Ghee</h3>Analysis by QuEChERS with GC/MS/MS using the Agilent 8890 GC and Agilent 7010 GC/TQ<ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_pesticide_ghee_gc_5994_8399en_agilent_1cbd787002.pdf">Full PDF for download</a></li></ul>India is one of the largest producers of milk, contributing about 23% of global milk production.1 The dairy processing sector includes a wide range of products, such as milk, butter, cheese, ghee, yogurt, flavored milk, lactose-free dairy products, and value-added products like ice creams and yogurts. Amongst these, ghee production is significant because of its popularity, low cost of production, and versatile use. According to the Food Safety and Standards Authority of India (FSSAI), ghee is mentioned as a "product obtained exclusively from milk, cream or butter by a process that almost completely removes water and non-fat solids; it has a specially developed flavor and physical structure".2 Milk‑producing animals can be exposed to pesticides through their diet, such as feed and fodder containing pesticide residues, or through the direct application of pesticides for controlling ectoparasites on their bodies, in animal sheds, and in milk processing areas. Due to their persistent and lipophilic nature, pesticides tend to accumulate in the fat-rich tissues of animals. The FSSAI has specified maximum residue levels (MRLs) for 55 pesticides, and a tolerance limit of 0.01&nbsp;mg/kg for the remaining pesticides for which an MRL has not been&nbsp;fixed.&nbsp;Ghee consists of 98.9% fat, irrespective of the animal source. Among the short- and medium-chain saturated fatty acids, all samples contain butyric (C4:0), caproic (C6:0), caprylic (C8:0), and capric acid (C10:0).3 Since its introduction, the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=QuEChERS">QuEChERS method</a> has been widely used for the analysis of pesticides in several matrices. Some modifications to the original QuEChERS method have been introduced to ensure efficient extraction of pH-dependent compounds, to minimize degradation of susceptible compounds (such as base- and acid-labile pesticides), and to expand the spectrum of matrices covered. Ghee matrix has a very high lipid load, making it a difficult commodity for analysis pesticide residues. The primary challenge lies in obtaining an extract that contains the target analytes while minimizing the amount of fat. Co-extracted lipids in the extracts can be removed, to a high degree, by a freezing-out step or a C18 cleanup.&nbsp;During sample extraction, the sample is often diluted. To obtain a quantification limit of 0.01 mg/kg, the instrument should be able to detect the residues at a lower concentration. This application note addresses these requirements by combining a sample preparation technique covering multiclass pesticides, target-specific multiple reaction monitoring (MRM) data acquisition, and efficient software to simplify quantitative analysis. The Agilent 7010 triple quadrupole GC/MS system enabled trace-level detection and confident quantitation of 150 pesticides in ghee.<h4>Experimental&nbsp;</h4><h5>Equipment&nbsp;</h5>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 <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=7010+GC%2FTQ">7010 GC/TQ</a> system equipped with high efficiency source was used for the analysis. The GC system was equipped with a multimode inlet with air cooling and midcolumn backflush based on an Agilent purged Ultimate union controlled by a pneumatic switching device. The method parameters are displayed in Table 1.<h4>Conclusion</h4>The limits of quantitation (LOQs) for the target list of over 150 compounds ranged from 2.5 to 5 mg/kg for the ghee matrix. To minimize interferences from the ghee matrix, numerous multiple reaction monitoring (MRM) transitions were employed. This approach helped to accurately identify and quantify the target compounds despite the complex sample matrix. The samples were diluted five-fold to ensure that the analytes were within the required detection range of the instrument. This dilution also helped in reducing the matrix effects, leading to more reliable results. The average analyte recoveries were between 70 and 130%, indicating that the method has good accuracy and precision. This range of recoveries demonstrates the method’s robustness and suitability for routine analysis of these compounds.<h3>2. EST Analytical: Analysis of Coffee Flavors by Purge and Trap Sampling</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_Analysis_of_Coffee_Flavors_by_Purge_and_Trap_Sampling_ca25beef60.pdf">Full PDF for download</a></li></ul>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.&nbsp;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.<h4>Experimental:&nbsp;</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 60m x 0.25mm x 1µm. Listed in Tables 1 and 2 are the experimental parameters used for this study.<h4>Conclusion:&nbsp;</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.<h3>3. Shimadzu: Analysis of Ethanol in E10 Gasoline Using Polyarc Microreactor for GC</h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_01_01033_en_d4ee66bd4f.pdf">Full PDF for download</a></li></ul>The flame ionization detector (FID) can detect almost all organic compounds, and the sensitivity of the obtained chromatograms displays a correlation with concentration and number of carbon atoms in the compound. However, as a weakness of FID, its sensitivity decreases when an organic compound contains oxygen atoms, asin the case of alcohols.&nbsp;The Polyarc microreactor improvessensitivity for alcohols and other compounds containing oxygen atoms (hereinafter, oxygenated compounds), allowing calibration using a single compound. Research and use of biofuels has accelerated in recent years, and more sensitive quantitative analysis of oxygenated compounds in multiple compoundsis now required.&nbsp;This Application News introduces an example of an analysis of a sample simulating E10 gasoline, in which 10 % ethanol by volume concentration was added to gasoline, demonstrating that enhanced sensitivity for oxygenated compounds can be achieved by adding Polyarc to the instrument configuration. The accuracy of the quantitative analysis was also verified using a general standard sample (alkane).<h4>Polyarc Microreactor</h4>Polyarc is a post-column type microreactor that is introduced between the column and the detector (FID). The organic compounds separated and eluted by the column are decomposed to methane by the Polyarc reactor in a two-stage oxidationreduction reaction (Fig. 1). Since the decomposed methane is detected by the FID, the uniform sensitivity for the carbon number can be obtained, regardless of the type of functional groups in a sample.<h4>Effective Carbon Number</h4>As mentioned above, the sensitivity of the FID detector varies depending on the types of functional groups in organic compounds. The detection sensitivity by the FID can be estimated based on the concept of the effective carbon number (ECN), which is an index showing how many carbon atoms in a compound function effectively. Depending on the type of functional groups contained in a compound, the carbon ratio in the molecule changes, and this causes changesin the sensitivity ofthe FID. For example, both ethane (C2H6) and ethanol (C2H5OH) contain the same number of carbon atoms of 2, but the sensitivity of the FID for ethanol is only 75 % of itssensitivity for ethane because the primary hydroxyl group (-OH) behaves as -0.5 carbon atoms in terms of its contribution to the ECN. This meansthe ECNof ethanol is 1.5. Table 1 shows several examples of other functional groups with ECNslowerthan the number of carbon atoms.<h4>Analysis Conditions</h4>In this Application News, sensitivity for ethanol when the Polyarc was added and when using only the FID was compared using an E10 sample, in which 10 v/v% ethanol was added to gasoline, simulating a biofuel which has attracted attention in recent years, and quantitativity for ethanol was confirmed. In the quantitative analysis, it was also carried out by the external standard method using a hydrocarbon (dodecane; C12) with a concentration of 1 w/v% as a standard sample. The analytical instrument was a <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=1&amp;search=GC-2030">GC-2030</a> (SPL/FID) model gas chromatograph with the Polyarc added (Fig. 2). Table 2 shows the analysis conditions.<h4>Conclusion</h4>E10 gasoline was analyzed using an FID detector and an added Polyarc microreactor, confirming that oxygenated compounds can be analyzed with high sensitivity. This study also confirmed that a uniform reaction of organic compounds can be obtained in the FID, and peak broadening can be suppressed by standardizing the response of sensitivity. Table 6 introduces several of the advantages that are possible by adding the Polyarc microreactor. The Polyarc converts all organic compounds to methane having the same number of carbon atoms (mol), enabling highsensitivity detection for compounds with low detection sensitivity by FID alone. In addition, since sensitivity is standardized, quantitation is possible using only one arbitrary calibration curve, regardless of the type of analysis compound. As a result, it is now possible to analyze compounds that were difficult to analyze by FID until now.

News from LabRulezGCMS Library - Week 47, 2025

<h4>Abstract&nbsp;</h4>The United States Environmental Protection Agency (USEPA) Method 8260 is used in order to ascertain volatile organic compounds in waters, soils and solid waste samples. Often times, soil and solid waste samples are so highly contaminated the sample needs to be dispersed in methanol. Sample collection for contaminated soils can be obtained in two ways. One, dispersing a bulk soil sample into a 40ml vial and adding methanol in the lab or two, sending preweighed vials with a septum sealed cap that already contains the pre-requisite methanol out in the field for soil sampling. No matter how the soil sample is dispersed in methanol, an aliquot of the methanol extract needs to be added to water and purged using USEPA Method 5030. This application will investigate automated sampling of methanol soil extractions.Introduction: 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.<h4>Experimental</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=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=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 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: 40mL/min</li><li>Dry Purge Time: 1.0 min &nbsp;</li><li>Desorb pressure Control: ON</li><li>Desorb Pressure: 6psi</li><li>Desorb time: 0.5 min</li><li>Desorb preheat delay: 15 sec</li><li>Desorb temperature: 260 °C</li><li>MoRT bake temperature: 210 °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: 85 mL/min</li></ul><h5>Purge and Trap Auto-Sampler: EST Centurion WS</h5><ul><li>Sample Type: Water</li><li>Water Volume: 5ml</li><li>Sample Prime Time: 5 sec</li><li>Loop Equilibration Time: 5 sec</li><li>Sample Transfer Time: 15 sec.</li><li>Syringe Rinse: On/6 ml</li><li>Number of Syringe Rinses: 2</li><li>Sample Loop Rinse: On/15 sec</li><li>Sample Sweep Time: 15 sec</li><li>Number of Sparge Rinses: On/2</li><li>Rinse Volume: 5 ml</li><li>Rinse Transfer Time: 15 sec</li><li>Rinse Drain Time: 25 sec</li><li>Internal Standard Vol.: 5 µl</li><li>Extraction: MeOH Prep A (Sand and Clay)</li><li>Extraction: MeOH Prep B (Potting Soil)&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/splitless mode, 220 °C, 40:1 split ratio, 12.153 psi inlet 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 15 °C/min → 220 °C, hold for 1.33 min, 14 min run time</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 35–300, 5.2 scans/sec</li><li>Solvent delay: 0.7 min</li></ul>The EPA method 8260 standards were acquired from Restek while the purge and trap grade methanol was procured from JTBaker. A nine point methanol curve was established from 0.5 to 200µg/L. Next Method Detection Limits (MDLs) were found running seven replicates of the low point on the curve. Precision and accuracy was determined by examining seven replicates of the 50µg/L standard. Table 3 displays the curve, MDL and precision and accuracy results. A set of three spiked sand matrix samples were used to establish the accuracy of the automated extraction at a 50µg/L concentration, see Table 4.<img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/EST_Analytical_Table_3_Curve_MDL_and_Precision_and_Accuracy_Results_38f2c858a9.jpg" alt="EST Analytical: Table 3 - Curve, MDL and Precision and Accuracy Results." srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_EST_Analytical_Table_3_Curve_MDL_and_Precision_and_Accuracy_Results_38f2c858a9.jpg 159w," sizes="100vw" width="1102" height="1083"><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/EST_Analytical_Table_4_Results_of_Automated_Extraction_of_a_Sand_Matrix_3874d74191.jpg" alt="EST Analytical: Table 4 - Results of Automated Extraction of a Sand Matrix" srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_EST_Analytical_Table_4_Results_of_Automated_Extraction_of_a_Sand_Matrix_3874d74191.jpg 91w," sizes="100vw" width="741" height="1267">Finally, sand, clay and soil matrices were extracted in order to compare the chromatography of the automated extractions using different matrices. The matrix comparison required 5 grams of soil and 15mls of methanol due to the potting soils’ absorption of the methanol. Thus, in order to make a direct comparison, all of the matrices were spiked with the same volume of standard and extracted with 15mls of methanol. Figure 1 displays a comparison of the three matrices and their respective interaction with the extraction solvent and Figure 2 shows the chromatograms of the three matrices.<img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/EST_Analytical_Figure_1_Image_of_5g_of_soil_matrices_in_15mls_of_Methanol_fc02a00c9d.jpg" alt="EST Analytical: Figure 1 - Image of 5g of soil matrices in 15mls of Methanol" srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_EST_Analytical_Figure_1_Image_of_5g_of_soil_matrices_in_15mls_of_Methanol_fc02a00c9d.jpg 185w," sizes="100vw" width="565" height="477"><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/EST_Analytical_Figure_2_Chromatograms_of_Automated_Extraction_of_Sand_Clay_and_Soil_53e50f4fc4.jpg" alt="EST Analytical: Figure 2 - Chromatograms of Automated Extraction of Sand, Clay and Soil" srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_EST_Analytical_Figure_2_Chromatograms_of_Automated_Extraction_of_Sand_Clay_and_Soil_53e50f4fc4.jpg 245w," sizes="100vw" width="1396" height="702"><h4>Conclusions</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.

Automated Sampling of Methanol Extractions 

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

News from LabRulezGCMS Library - Week 48, 2025

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

News from LabRulezGCMS Library - Week 49, 2025

<h4>Abstract</h4>Desorb flow control was developed in order to help manage the moisture associated with the four minute desorb time required for USEPA method 524.2. An added benefit to this process is the reduction in helium consumption when using this technique. This application will explain the patented process of Desorb Flow Control (DFC) (United States Patent Office numbers: 8062905, 7951609, 7803635) for Helium conservation and moisture control.&nbsp;<h4>Introduction</h4>Helium has been an essential component in environmental testing for years. Since Helium is an inert gas with a similar diffusion speed as Hydrogen, it is ideal for using as a carrier gas in Gas Chromatography. In recent years, however, there has been an increasing shortage of Helium, leading laboratories to come up with different ways of conservation.&nbsp;Desorb Flow Control was developed to assist laboratories routinely running for USEPA Method 524.2. Method 524.2 requires a four minute desorb and laboratories are reporting issues with water when using the long desorb time. By using DFC, labs are now able to keep the required four minute desorb time and control the amount of water transferred to the GC by decreasing the flow through the trap during desorb while maintaining the desired split ratio at the GC inlet. Subsequently, DFC not only controls the amount of water transferred, but also decreases Helium consumption. See Figures 1 and 2.<img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/EST_Analytical_Figure_1_Traditional_GC_Flow_ebb2a6357c.jpg" alt="EST Analytical: Figure 1 - Traditional GC Flow" srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_EST_Analytical_Figure_1_Traditional_GC_Flow_ebb2a6357c.jpg 245w," sizes="100vw" width="1106" height="553"><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/EST_Analytical_Figure_2_GC_Flow_with_Encon_Evolution_using_DFC_5af219d179.jpg" alt="EST Analytical: Figure 2 - GC Flow with Encon Evolution using DFC" srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_EST_Analytical_Figure_2_GC_Flow_with_Encon_Evolution_using_DFC_5af219d179.jpg 245w," sizes="100vw" width="1389" height="684"><blockquote>(NOTE: The Encon Evolution provides the increased flow after the trap during desorb at a set time in the desorb process.)&nbsp;</blockquote>The advent of more efficient purge and trap systems and more sensitive GC/MS systems has aided in laboratories’ production. However, water control is still an issue. Labs may pass an initial calibration curve, but as water builds up in the system, internal standard response drops over time, causing the laboratory to fail continuing calibration checks. In order to combat water, many labs use a high split rate. As a consequence, Helium consumption is much higher and sensitivity is decreased. Using DFC, labs can still achieve the moisture control required thus creating a more stable system and lowering Helium consumption by as much as 80%, depending on the experimental split rate. See Table 1. *The table below assumes a throughput of 72 samples per day.<img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/EST_Analytical_Table_1_Daily_Helium_Consumption_ee240f3668.jpg" alt="EST Analytical: Table 1 - Daily Helium Consumption" srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_EST_Analytical_Table_1_Daily_Helium_Consumption_ee240f3668.jpg 245w," sizes="100vw" width="1454" height="323"><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 Encon 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=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">5975C inert XL MS</a>. The GC was configured with a Restek Rxi-624 Sil MS 30m x 0.25mm x 1.4µm column. Two different split ratios were used for comparison in this study, a 40:1 split rate was used for the baseline data and a 10:1 split rate was used for the DFC data. Experimental parameters used for this analysis 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: 40mL/min</li><li>Dry Purge Time: 1.0 min &nbsp;</li><li>Desorb pressure Control: ON</li><li>Desorb Pressure: 13.5 psi</li><li>Desorb time: 4.0 min</li><li>Desorb preheat delay: 10 sec</li><li>Desorb temperature: 250 °C</li><li>MoRT bake temperature: 210 °C</li><li>Bake temperature: 260 °C</li><li>Sparge vessel bake temperature: 110 °C</li><li>Bake time: 8 min</li><li>Bake flow: 85 mL/min</li></ul><h5>Purge and Trap Auto-Sampler: EST Centurion WS</h5><ul><li>Sample Type: Water</li><li>Water Volume: 25ml</li><li>Internal Standard Vol.: 5 µl</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 7890A/5975</a></li><li>Inlet: Split/splitless mode, 200 °C, 40:1 and 10:1 split ratio, 7.45 psi inlet head pressure</li><li>Column: Rxi-624Sil MS 30m x 0.25mm I.D. 1.4µm film thickness</li><li>Oven program: 40 °C (1.5 min) → ramp 8 °C/min → 100 °C, ramp 20 °C /min to 210 °C, hold for 1.25 min, 16.5 min run time</li><li>Column flow rate: 1 mL/min helium</li><li>Total flow: 13.8 and 43.8 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 35–300, 3.12 scans/sec</li><li>Solvent delay: 1.0 min</li></ul>The USEPA Method 524.2 standards were acquired from AccuStandard. The linear ranges of the experiments were established by running eight point calibration curves from 0.5 to 100ppb. Table 4 displays curve linearity and compound response for the curves. Figure 3 displays chromatograms of the 20ppb calibration point with and without DFC. Finally, an experiment was run using Selective Ion Monitoring (SIM) of m/z 20 with and without DFC. This was done in order to show water control using D2O as the compound of interest so as not to SIM for water and overwhelm the MS. Figure 4 displays the results of this experiment.<img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/EST_Analytical_Table_4_Curve_Linearity_and_Compound_Response_Summary_7303558674.jpg" alt="EST Analytical: Table 4 - Curve Linearity and Compound Response Summary" srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_EST_Analytical_Table_4_Curve_Linearity_and_Compound_Response_Summary_7303558674.jpg 107w," sizes="100vw" width="684" height="1003"><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/EST_Analytical_Figure_3_20ppb_Chromatograms_With_and_Without_DFC_bebdb4c00f.jpg" alt="EST Analytical: Figure 3 - 20ppb Chromatograms With and Without DFC" srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_EST_Analytical_Figure_3_20ppb_Chromatograms_With_and_Without_DFC_bebdb4c00f.jpg 245w," sizes="100vw" width="1383" height="518"><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/EST_Analytical_Figure_4_Overlay_of_D2_O_mz_20_With_and_Without_DFC_701bb4011c.jpg" alt="EST Analytical: Figure 4 - Overlay of D2O mz 20 With and Without DFC" srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_EST_Analytical_Figure_4_Overlay_of_D2_O_mz_20_With_and_Without_DFC_701bb4011c.jpg 143w," sizes="100vw" width="939" height="1026"><h4>Conclusions</h4>The results of this study show the patented Desorb Flow Control is an exceptional tool for conserving helium and creating a more stable system. The option of maintaining the desired split ratio at the GC inlet while decreasing the flow through the trap during desorb provides sensitivity while controlling the amount of moisture being sent onto the GC column. Furthermore, the split rate during the GC/MS run time is substantially lower than during the desorb time. Laboratories can have the advantage of running a higher split rate during the desorb process then maintaining a lower split during the rest of the GC/MS separation and analysis, thus providing laboratories with up to an 80% reduction in GC/MS helium use.

Benefits of Using Desorb Flow Control with the Encon Evolution

Our Library never stops expanding. What are the most recent contributions to LabRulezGCMS Library in the week of 8th December 2025? Check out new documents from the field of the gas phase, especially GC and GC/MS techniques!<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 Thermo Fisher Scientific and other document by Shimadzu!<h3>1. Agilent Technologies: High-Precision Determination of Four Greenhouse Gases in the Atmosphere Using the Agilent 8890 GC</h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_monitoring_greenhouse_gas_8890_gc_5994_8744en_agilent_0e08f0909f.pdf">Full PDF for download</a></li></ul>Currently, China is actively implementing dual-control measures on total energy consumption and intensity. The Ministry of Ecology and Environment issued "The 14th Five-Year Plan for Ecological and Environmental Monitoring", which specifically highlights the advancement of technologies for direct measurement of carbon emissions. It calls for organizing pilot projects in multiple key industries and enterprises to monitor greenhouse gas emissions such as carbon dioxide and methane, establishing greenhouse gas monitoring networks in key cities, and upgrading the greenhouse gas monitoring capabilities of national atmospheric background stations. As a result, conducting greenhouse gas monitoring within the environmental protection stations of provinces and cities has become a critical task.The use of GC for detecting greenhouse gases has a long history. The conventional methods used gas sampling valve for injection, TCD and FID for sequential detection of CO2 and CH4 , or combining a methanizer with an FID to detect CO2 and CH4 in one analytical channel and detecting N2O on ECD in another analytical channel.2 The analytical precision for CO2, CH4, and N2 O achieved with such configurations typically ranges from 0.2% to 0.5%, but it is difficult to obtain precision better than 0.1%, which does not meet the current requirements for greenhouse gas monitoring accuracy and precision. Moreover, the traditional methods rarely report analytical precision for SF6 at ppt concentration levels. To monitor trace levels of CO2 , CH4, N2O, and ultratrace levels of SF6 on the same GC system with high-precision results, it is necessary to optimize multiple factors included in sample injection, separation, and detection. Furthermore, the system configuration must be flexible enough to allow expansion for future analytical needs, such as incorporating trace CO analysis in air. This work demonstrates how the 8890&nbsp;GC achieves high-precision analysis of four key greenhouse gases by optimizing the injection volume, controlling injection reproducibility, and utilizing multichannel separation and high-sensitivity detectors to ensure the system runs stably in long‑term operation.<h4>Experimental</h4><h5>Instrumental&nbsp;</h5>The <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=1&amp;search=8890+GC">8890 GC</a> is configured as a three-channel/multivalve/multicolumn system, enabling independent analysis of four greenhouse gases—CH4 , CO2 , N2O, and SF6 —within 8 minutes using a single injection. The target compounds are analyzed in separate channels, reducing chromatographic peak broadening and thereby improving sensitivity and&nbsp;repeatability.&nbsp;<ul><li>For CO2 analysis, a <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=1&amp;search=methanizer">methanizer</a> is used to convert CO2 to CH4 , which is then detected by FID. The system eliminates the need for dehydration through backflushing and venting operation via switching valves, preventing interference from moisture and oxygen in the air and extending the lifespan of the methanizer.&nbsp;</li><li>For N2O and SF6 analysis, the ECD with hidden anode design is used for high‑sensitivity detection and strong anti‑contaminant capability.&nbsp;</li><li>The CH4 analysis is conducted on a single column with a dedicated large injection loop, significantly enhancing detection sensitivity and repeatability, achieving a detection limit for methane as low as single-digit ppb levels.</li></ul><h4>Conclusion&nbsp;</h4>Based on its exceptional pneumatic control and valve-based flow path design, the multivalve/multicolumn Agilent 8890 GC system achieves high-sensitivity and high-precision measurements of four key greenhouse gases. This is accomplished through optimized and precise control of sample flow rate/volume, selection of premium analytical columns, and the use of highly stable and robust FID and ECD. Standard gas samples of CO2 , CH4 , N2 O, and SF6 , with concentrations equivalent to atmospheric levels, were measured continuously 10 times. The measurement precision for these gases was better than 0.05%, 0.1%, 0.1%, and 0.5%, respectively, fully meeting the high-precision monitoring requirements of environmental monitoring stations at various levels for target greenhouse gases. Compared to other monitoring solutions, this approach is based on a stable and reliable gas chromatography platform that is technically easier to master and deploy. It represents a trusted solution developed by Agilent to assist in establishing a greenhouse gas monitoring network in China.<h3>2. Shimadzu: GC/MS Mass Spectra Library - Polymer Additives Library Ver.2</h3><ul><li>Other document</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/c146_e506_d4c93c4d60.pdf">Full PDF for download</a></li></ul><h4>Contains Approximately 5,800 Mass Spectra&nbsp;</h4>This library consists of a library*, which contains 5,775 mass spectra for 590 types of polymer additives and GC/MS pyrolysates from the pyrolysis GC/MS analysis of additives, and a library containing the mass spectra for 65 compounds often targeted for analysis, selected based on their usage in the commercial market, and chemical substance regulatory information. In total, this product contains 5,840 mass spectra, which provides strong support for the analysis of polymer additives. In Ver.2, the compound registration has been newly enhanced, for example vulcanizing accelerators utilized in the rubber filed. Approximately 1,000 spectra have been added.&nbsp;*ADD-MS22B F-Search Additives Library from Frontier Laboratories<h4>Can Be Used with a Variety of GC/MS Systems&nbsp;</h4>The library can be used for a variety of GC/MS applications, including pyrolysis GC/MS, which is widely used for the analysis of additives in polymer materials, and liquid sample injection GC/MS. It supports a wide range of additive analysis for customers.<h4>Library Specifications</h4><ul><li>Registered compounds: 5,775+65&nbsp;</li><li>Registered information: Mass spectrum, retention index for each analytical condition, compound name, molecular weight, compositional formula, structural formula, classification of additives</li><li>Applicable models: <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=3&amp;search=GCMS-QP2050">GCMS-QP™ serie</a>s, <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=3&amp;search=GCMS-TQ8050">GCMS-TQ™ series</a> (This library does not include MS/MS spectra.)&nbsp;</li><li>Pyrolyzer (Pyrolysis analysis system): <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=43&amp;search=PY-2020D">PY-2020D</a>, <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=43&amp;search=PY-2020iD">PY-2020iD</a>, and <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=43&amp;search=EGA%2FPY-3030D">EGA/PY-3030D</a></li><li>Workstations: <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=3&amp;search=GCMSsolution">GCMSsolution</a>™ Ver. 4.6 and later, <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=3&amp;search=LabSolutions+GCMS">LabSolutions™ GCMS</a>™ Ver. 5.131 and later, LabSolutions DB/CS GCMS Ver. 6.131 and later</li></ul><h3>3. Thermo Fisher Scientific: Trace analysis of epichlorohydrin in drinking water using GC-MS coupled with 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/an_003894_gc_single_quad_isq_7610_environmental_an003894_na_en_70123385ae.pdf">Full PDF for download</a></li></ul>Epichlorohydrin (ECH) is a versatile starting material in the production of drugs and polymers and is also used as an insect fumigant and solvent for organic synthesis reactions. ECH-based polymer pipes are commonly used in the production of drinking water due to their durability and resistance to corrosion. However, ECH is known for its high reactivity and toxicity, which poses significant health risks if it contaminates drinking water. Exposure to ECH can cause respiratory issues, skin irritation, and has been classified as a probable human carcinogen.1Due to these risks, many countries have imposed strict limits on the amount of ECH allowed in drinking water. Recently, Europe set a minimum detection limit (MDL) of 30 parts per trillion (ppt) for ECH in drinking water.2 Whereas typically required detection limits for most compounds mandated for analysis in Europe can be achieved using methods based on static headspace, the stringent MDL required for ECH requires preconcentration, for example using purge and trap (P&amp;T) technology.3,4 This technology involves purging the water sample with an inert gas to release volatile organic compounds (VOCs), which are then trapped and concentrated for analysis, ensuring reliable detection at very low concentrations. In the United States, the analysis of VOCs in drinking water is mandated by the Environmental Protection Agency (EPA). The EPA requires the use of P&amp;T technology for drinking water analysis to ensure that even trace amounts of harmful compounds like ECH are detected and managed appropriately.&nbsp;The following evaluation describes the use of the ISQ 7610 Single Quadrupole MS system coupled with the Thermo Scientific™ TRACE™ 1610 GC with the Thermo Scientific™ HeSaver-H2 Safer™ split/splitless injector and Teledyne LABS Tekmar Lumin P&amp;T concentrator combined with the AQUATek LVA autosampler for the analysis of ECH in drinking water.<h4>Experimental</h4><h5>GC-MS parameters&nbsp;</h5>A <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/486">TRACE 1610 GC</a> was coupled to the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/484">ISQ 7610 MS</a> equipped with the Thermo Scientific™ NeverVent ™ vacuum probe interlock (VPI) and an ExtractaBrite ion source. A <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/1773">Thermo Scientific™ TraceGOLD™ TG-VMS column</a>, 30 m × 0.25 mm, 1.4 µm film (P/N 26080-3320) was used for compound separation. The HeSaver-H2 Safer SSL injector was utilized to reduce the carrier gas consumption by decoupling the gas used for the chromatographic separation from the gas used to pressurize the inlet and maintain split and purge flows. The critical separations were maintained with a run time of under 15 minutes.For this analysis, the ISQ 7610 MS was operated in Selected Ion Monitoring (SIM) mode for increased selectivity, as required for this application. Extended method parameters for the ISQ 7610 MS are shown in Table 2.<h5>Instrument control and data processing&nbsp;</h5>Data was acquired, processed, and reported using the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/76">Thermo Scientific™ Chromeleon™ Chromatography Data System (CDS)</a>. This software can control both the GC-MS system and the Tekmar Lumin P&amp;T with the AQUATek LVA. This allows a single software to be utilized for the full workflow, simplifying the instrument operation. This application note is available for download via the Thermo Scientific™ AppsLab Library, which contains all the parameters needed to acquire, process, and report the analytical data for analysis of ECH.5<h4>Conclusion&nbsp;</h4>This study demonstrates the capability of the Tekmar Lumin P&amp;T with the AQUATek LVA system connected to the ISQ 7610 Single Quadrupole GC-MS to detect and quantify low-level ECH in drinking water samples, in compliance with EPA requirements.&nbsp;<ul><li>Utilizing the Tekmar Lumin P&amp;T’s ability to purge with nitrogen, along with using the HeSaver-H₂Safer SSL injector, nearly four times less helium was consumed during the analysis without sacrificing system performance.&nbsp;</li><li>The linearity of the calibration curve from 30 ppt to 5,000 ppt passed method requirements.</li><li>The application proved robust during an extended study with 20 samples of a 1,000 ppt ECH standard injected over a series of 124 injections, obtaining 4.4% precision and 118% accuracy of the recovery.</li></ul>

News from LabRulezGCMS Library - Week 50, 2025

Our Library never stops expanding. What are the most recent contributions to LabRulezGCMS Library in the week of 15th December 2025? Check out new documents from the field of the gas phase, especially GC and GC/MS techniques!<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, Shimadzu and brochure by Thermo Fisher Scientific!<h3>1. Agilent Technologies: Increased Thermal Stability of the DB‑5Q GC Column</h3>Increased signal-to-noise for trace level concentrations of controlled substances<ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_stability_gc_column_5994_8658en_agilent_4c52ae52cf.pdf">Full PDF for download</a></li></ul>The analysis of controlled substances by gas chromatography/mass spectrometry (GC/MS) requires a high level of confidence and thus requires a method that provides optimal data quality. Identification of controlled substances relies heavily on comparison of mass spectra to commercially available spectral libraries, and increased column bleed can cause spectral interference at high temperatures. These interferences can lead to poor library matching probabilities.1-3 The <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=J%26W+5Q">Agilent J&amp;W 5Q series</a> of gas chromatography columns provide the most thermally stable columns available, which helps to decrease spectral interference due to column bleed and improves data accuracy.&nbsp;Poor thermal stability will cause an increase in the slope of the baseline as the oven temperature is increased, leading to difficult peak integrations and inaccurate quantitation. Additionally, sloped or elevated baselines can lead to a decreased response and a loss of sensitivity for analytes eluting during the oven ramp or at the method’s upper temperature limits. Several commercially available 5ms type columns were compared to the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=J%26W+DB-5Q">Agilent J&amp;W DB-5Q GC column</a> to examine the impact thermal stability has on response at upper temperature limits.&nbsp;<h4>Experimental&nbsp;</h4>An <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=8890+GC">Agilent 8890 GC system</a> coupled with an <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=5977B">Agilent 5977B mass selective detector (GC/MSD)</a> with an inert extractor ion source was used for acquisition of data and MassHunter 10.0 Quantitative and Qualitative Analysis software was used for data analysis.&nbsp;A representative toxicology mixture, the Agilent GC/MS forensic toxicology checkout mixture (part number 5190-0471) was used to monitor analytical performance. Calibration standards were prepared in methanol (MeOH) at concentrations ranging from 0.1 to 3.0&nbsp;μg/mL. An internal standard mix was prepared at 10&nbsp;μg/mL from individual stocks of methamphetamine-d3, diazepam-d5, and hydrocodone-d6 all purchased from Millipore Sigma (St.&nbsp;Louis, MO).<h4>Results and discussion&nbsp;</h4>The testing evaluated the Agilent J&amp;W DB-5Q GC column for the analysis of controlled substances by GC/MS. The increased thermal stability of the DB-5Q is seen in the decreased baseline at higher temperatures, as seen in Figure&nbsp;1, and also provides a decrease in the slope during the oven ramping program.&nbsp;An increase in the slope of the baseline will also decrease the signal-to-noise ratio (S/N) of an analyte but will also make integration more difficult and lead to less accurate quantitative results. Figure 2 demonstrates the comparison of the DB-5Q and the commercially available 5ms type G column, and the impact to chromatography during the oven ramp. The S/N for the analytes on the oven ramp slope are a factor of ten or greater for the DB-5Q in comparison to the 5ms type G column.<h4>Conclusion&nbsp;</h4>The increased thermal stability of the Agilent J&amp;W DB-5Q GC column demonstrated in this application note provides a decreased baseline at higher temperatures, which allows for an increased response for later eluting compounds at trace level concentrations. The baseline of the DB-5Q remains more consistent as the temperature is increased. This consistency allows for more accurate integration and quantitation for analytes eluting during oven ramping, in comparison to other commercially available 5ms-type columns. The robust DB-5Q column phase maintained peak shape for trace level basic compounds even when stressed with a heavy matrix and is an excellent choice for the analysis of controlled substance&nbsp;analysis.<h3>2. Shimadzu: Quantitative Analysis of Anti-Degradant Additive (6PPD) in Tire Rubber Using Pyrolysis-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_00952_en_b95b2348e5.pdf">Full PDF for download</a></li></ul><h5>User Benefits</h5><ul><li>The simple analysis procedure required just cutting off a sample fragment and placing it in a sample cup without pretreatment.</li><li>Utilizing a calibration standard that includes a resin solution allows for analysis under conditions that closely resemble those of samples, which improves the reliability of quantitative measurements.</li><li>With Shimadzu’s Polymer Additive Library, it is possible to acquire information on the additives of identified compounds.</li></ul>6PPD (N-(1,3-dimethylbutyl)-N'-phenyl-p-phenylenediamine) is an anti-degradant (anti-oxidant) additive that is used in many rubber products. Its chemical structure is shown in Fig. 1. It plays an important role in tires by preventing degradation and extending its lifespan. However, when 6PPD reacts with ozone in the atmosphere, it forms a highly toxic substance called 6PPD-quinone (6PPD-Q).&nbsp;As an automotive tire wears, microscopic particles are released from the tire into the environment. These particles, tire road wear particles (TRWP), contain 6PPD-Q along with many other chemical substances. On rainy days, these particles are washed into rivers and other bodies of water, where they accumulate in the environment as microplastics.&nbsp;There are serious concerns about the negative effects these microplastics have on ecosystems and the environment. 6PPDQ has been shown to induce acute mortality in Salmonidae fish, specifically coho salmon. 1)&nbsp;Currently, there is no commercial alternative that can maintain tire stability and performance with minimal impact on the environment. Research into alternatives requires accurately assessing 6PPD levels in rubber products and objectively determining whether alternative compounds offer equivalent stability and performance while having a reduced impact on the environment.&nbsp;This article describes using a pyrolysis gas chromatograph mass spectrometer (Py-GC-MS) system to measure 6PPD levels in tire rubber.<h4>Analysis Process&nbsp;</h4>ISO/TS 21396describes a method for determining the mass concentration of TRWP in soil and sediment that uses Py-GC-MS. Similar to this method, Py-GC-MS was used for the analysis; however, this article employs optimized analytical conditions. A schematic diagram of the analysis processisshown in Fig. 2. For more information on the analysis conditions and results from the evolved gas analysis (EGA-MS, <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=42&amp;search=EGA%2FPY-3030D">EGA/PY-3030D Multi-Shot Pyrolyzer AS-1020E Auto-Shot Sampler</a>, Frontier Laboratories Ltd.) method described in Fig. 2, please see Application News No. 01-00901. The analysis conditions for the thermal desorption (TD)-GC/MS (<a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=1&amp;search=GCMS-QP2020+NX">GCMS-QP2020 NX</a>) method used in this article are shown in Table 1. The thermal desorption temperature was chosen based on results obtained by the EGA-MS method.<h4>Qualitative Analysis of Additive&nbsp;</h4>The total ion current (TIC) chromatogram obtained from analyzing the tire rubber is shown in Fig. 4. A spectral library search was also performed using NIST-23 and Shimadzu’s Polymer Additives Library. The library search results for the peak that eluted at around 10.43 minutes are shown in Fig. 5. Based on the results from Shimadzu’s Polymer Additives Library, the peak was estimated to be the anti-degradant Nocrac 6C (a trade name for the chemical 6PPD).<h4>Conclusion&nbsp;</h4>This article presents an analysis of the additive 6PPD in tire rubber utilizing Py-GC-MS. Good results were obtained for calibration curve linearity, calibration standard repeatability, limit of quantification, and limit of detection. Shimadzu’s Polymer Additives Library was used to identify the additive.<h3>3. Thermo Fisher Scientific: Gas chromatography analyzers for the oil &amp; gas industry: upstream to downstream</h3><ul><li>Brochure</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/br_003966_gc_analyzers_trace_1610_industrial_br003966_na_en_44ad1327c6.pdf">Full PDF for download</a></li></ul>Gas chromatography (GC) plays a central role in the oil and gas industry, providing high-accuracy, high-speed analysis of complex hydrocarbon mixtures from upstream exploration through midstream transport to downstream refining and distribution. Across this value chain, GC supports regulatory compliance, product quality control, custody transfer, and process optimization. As the industry adapts to decarbonization goals and stricter environmental regulations, robust and automated analytical solutions have become essential for monitoring hydrocarbons, impurities, and trace components under demanding 24/7 operational conditions.Thermo Scientific™ GC analyzers are engineered to meet these challenges, with the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/486">TRACE™ 1610 GC</a> platform forming the backbone of a comprehensive portfolio of preconfigured and customizable systems. Its modular “Instant Connect” design enables rapid configuration of injectors, detectors, and valves, reducing downtime and simplifying maintenance. The platform supports multi-detector configurations—including FID, TCD, FPD, PDD, MS, and VUV—allowing a single analyzer to address a broad range of applications, from natural gas composition and BTU determination to sulfur species, fixed gases, and detailed hydrocarbon analysis .Dedicated GC analyzer configurations are available for specific industry needs, including natural gas and natural gas liquids (NGA/NGL), refinery gas analysis (RGA), light hydrocarbons (LPG), oxygenates, aromatics (BTEX), permanent gases, and high-purity gas streams. Advanced techniques such as GC-VUV further simplify complex analyses like PIONA group-type characterization of gasoline, delivering comprehensive compositional data in a single run while reducing calibration effort and cost per sample. These systems are designed to comply with major ASTM, ISO, GPA, DIN, EN, and UOP standards, ensuring global regulatory alignment .Complementing the hardware, <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/76">Thermo Scientific™ Chromeleon™ Chromatography Data System (CDS)</a> provides an integrated informatics backbone for method control, data processing, reporting, and connectivity to LIMS platforms. This unified approach enhances data integrity, improves workflow efficiency, and enables real-time decision-making across refinery and gas processing operations. Together, Thermo Scientific GC analyzers and integrated software solutions deliver reliable, scalable, and future-ready analytics for the evolving oil and gas industry.

News from LabRulezGCMS Library - Week 51, 2025

For more than 30 years, oxygenated compounds have been added to gasoline. The use of oxygenates provides two primary benefits: a reduction in pollution caused by vehicle emissions, as oxygenated gasoline burns more efficiently, and an improvement in overall engine performance.However, the prolonged use of oxygenated compounds has also led to environmental concerns. Increased contamination of groundwater has been observed, primarily due to leaks from underground storage tanks, allowing oxygenates to migrate into soil and water. In addition, because these compounds are highly soluble in water, analytical methods must be carefully optimized to achieve adequate detection limits.<h4>Discussion</h4>This application note investigates purge-and-trap experimental conditions to determine the most efficient and accurate approach for purging highly soluble fuel oxygenates. The study focuses on evaluating the effects of sample volume and purge temperature on analytical performance.The parameters examined include purge volumes of 5 mL, 10 mL, and 25 mL, as well as purge temperatures at room temperature and 60 °C. Experimental results were compared in terms of calibration range, linearity, method detection limits (MDLs), and compound response.A key feature of this study is the use of the EST Encon Evolution purge-and-trap concentrator, which provides enhanced control over moisture introduction into the GC system. Unlike conventional concentrators, the Encon Evolution employs an 8-port valve design that transfers analytes directly from the analytical trap to the GC via the transfer line, while excluding the Moisture Reduction Trap (MoRT) from the desorption pathway. This design is particularly advantageous when operating at elevated purge temperatures, as was required in this study. Flow paths for purge and desorption are illustrated in Figures 1 and 2.<img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/EST_Analytical_Purge_and_Desrob_Flow_Path_f7c9fec3a8.jpg" alt="EST Analytical: Figure 1 &amp; 2: Purge and Desrob Flow Path" srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_EST_Analytical_Purge_and_Desrob_Flow_Path_f7c9fec3a8.jpg 245w," sizes="100vw" width="1141" height="568"><h4>Experimental</h4><h5>Instrumentation</h5>The sampling and concentration system consisted of an <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/2159">EST Analytical Centurion WS autosampler</a> coupled to an <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/2160">EST Encon Evolution purge-and-trap concentrator</a>. Experiments were conducted in water mode.The concentrator was configured with a VOCARB 3000 trap and interfaced to an <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=7890A">Agilent 7890A gas chromatograph</a> equipped with a <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=5975C">5975 inert XL mass spectrometer</a>. GC/MS operating parameters were selected to support EPA Method 8260 analysis.<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: 12 psi</li><li>Desorb time: 1.0 min</li><li>Desorb temperature: 250 °C</li><li>MoRT bake temperature: 150 °C</li><li>Bake temperature: 265 °C</li><li>Sparge vessel bake temperature: 130 °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 7890A/5975</a></li><li>Inlet: Split/splitless mode, 200 °C, 40:1 split ratio, 17.311 psi inlet head pressure</li><li>Column: Rtx-624 20m x 0.18mm I.D. 1µm 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: 0.8 mL/min helium</li><li>Total flow: 38.8 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><h4>Standards and Calibration</h4>Oxygenate standards were obtained from Restek. The California oxygenate mixture included:<ul><li>Diisopropyl ether (DIPE)</li><li>Ethyl tert-butyl ether (ETBE)</li><li>tert-Amyl methyl ether (TAME)</li><li>tert-Butyl alcohol (TBA)</li><li>Methyl tert-butyl ether (MTBE)</li></ul>Most ether compounds were prepared at 2000 µg/mL, while TBA was prepared at 10,000 µg/mL. Ethanol standards were also obtained from Restek at 10,000 µg/mL.Calibration curves consisted of nine concentration levels, ranging from 0.5 to 200 ppb for ether compounds and 2.5 to 1000 ppb for TBA and ethanol. Method detection limits were determined using seven replicate injections at low calibration levels.<h4>Results and Discussion</h4>Evaluation of purge volume and purge temperature demonstrated that increasing sample volume resulted in improved compound response. Additionally, the use of a heated purge at 60 °C significantly enhanced the response of polar compounds, particularly ethanol and TBA, with ethanol response more than doubling under heated purge conditions.<img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/EST_Analytical_Table_3_Sample_Volume_and_Temperature_Experimental_Results_Summary_ace694091d.jpg" alt="EST Analytical: Table 3: Sample Volume and Temperature Experimental Results Summary" srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_EST_Analytical_Table_3_Sample_Volume_and_Temperature_Experimental_Results_Summary_ace694091d.jpg 245w," sizes="100vw" width="1600" height="372">While larger sample volumes generally increased sensitivity, the 10 mL sample volume combined with a 60 °C purge temperature provided the best balance of sensitivity, linearity, and chromatographic performance. This condition also produced the most consistent linear calibration range, especially for ethanol, which is traditionally difficult to analyze using purge-and-trap techniques.Chromatograms comparing room-temperature purge and heated purge conditions (Figures 3 and 4) clearly illustrate the improved peak response and signal stability achieved with heated purging.<img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/EST_Analytical_Figure_3_50ppb_Chromatogram_with_Room_Temperature_Purge_8ea1cd120f.jpg" alt="EST Analytical: Figure 3: 50ppb Chromatogram with Room Temperature Purge" srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_EST_Analytical_Figure_3_50ppb_Chromatogram_with_Room_Temperature_Purge_8ea1cd120f.jpg 245w," sizes="100vw" width="1548" height="688"><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/EST_Analytical_Figure_4_50ppb_Chromatogram_with_60_C_Purge_5246c294e6.jpg" alt="EST Analytical: Figure 4: 50ppb Chromatogram with 60 °C Purge" srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_EST_Analytical_Figure_4_50ppb_Chromatogram_with_60_C_Purge_5246c294e6.jpg 245w," sizes="100vw" width="1513" height="773"><h4>Full 8260 and California Oxygenate Analysis</h4>Following optimization, a full EPA Method 8260 calibration and validation was performed using the selected conditions (10 mL sample volume, 60 °C purge). Method performance was evaluated for linearity, precision (%RSD), recovery, and detection limits across the complete compound list.<img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/EST_Analytical_Table_4_Summary_of_8260_and_California_Oxygenate_Data_614adf67d6.jpg" alt="EST Analytical: Table 4: Summary of 8260 and California Oxygenate Data" srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_EST_Analytical_Table_4_Summary_of_8260_and_California_Oxygenate_Data_614adf67d6.jpg 211w," sizes="100vw" width="1600" height="1187"><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/EST_Analytical_Figure_5_50ppb_Standard_of_8260_and_Fuel_Oxygenates_5edd5bd337.jpg" alt="EST Analytical: Figure 5: 50ppb Standard of 8260 and Fuel Oxygenates" srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_EST_Analytical_Figure_5_50ppb_Standard_of_8260_and_Fuel_Oxygenates_5edd5bd337.jpg 245w," sizes="100vw" width="1219" height="560"><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/EST_Analytical_Figure_6_Extracted_Ion_Chromatogram_of_the_50_ppb_Standard_of_the_Fuel_Oxygenate_Compounds_in_the_8260_Mix_1e1684dbca.jpg" alt="EST Analytical: Figure 6: Extracted Ion Chromatogram of the 50 ppb Standard of the Fuel Oxygenate Compounds in the 8260 Mix" srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_EST_Analytical_Figure_6_Extracted_Ion_Chromatogram_of_the_50_ppb_Standard_of_the_Fuel_Oxygenate_Compounds_in_the_8260_Mix_1e1684dbca.jpg 245w," sizes="100vw" width="1188" height="561">Results demonstrated that the system met or exceeded all method performance criteria. Recoveries and precision were within acceptable limits for both volatile organic compounds and oxygenates, confirming suitability for regulatory compliance applications.<h4>Conclusions</h4>Overall, fuel oxygenate compounds exhibited higher responses with increased sample volume, while purge temperature had the greatest impact on polar analytes, particularly ethanol and TBA. The heated purge at 60 °C, combined with a 10 mL sample volume, produced optimal linearity and sensitivity.The EST Encon Evolution purge-and-trap system, equipped with a Moisture Reduction Trap (MoRT), proved to be highly effective for fuel oxygenate analysis. The system demonstrated excellent moisture control, robust analyte transfer, and reliable performance for both California oxygenates and full EPA 8260 compound lists. In all cases, method performance met or exceeded regulatory requirements.

California Oxygenates and 8260

Our Library never stops expanding. What are the most recent contributions to LabRulezGCMS Library in the week of 22nd December 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, EST Analytical and Shimadzu!<h3>1. Agilent Technologies: Analysis of Ethylene or Propylene Stream Cracking Gas Products</h3>Using the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=990+micro">Agilent 990 Micro GC</a><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_ethylene_propylene_stream_cracking_gas_products_5994_8803en_agilent_0cfe53e8f7.pdf">Full PDF for download</a></li></ul>Ethylene or propylene cracking gas products are produced from various feedstocks, including naphtha, light naphtha, atmospheric diesel, depressurized diesel, hydrotreating tail oils, ethane, and liquefied petroleum gas, among others.&nbsp;During gas cracking, yields of ethylene or propylene products should be monitored to measure the effectiveness of the process. The results of these analyses provide important process control data for optimizing cracking production and improving cracking yield—a key process parameter for cracking plants. Common cracking gas products are composed of hydrogen (H2 ), nitrogen (N2), and light hydrocarbons such as ethylene (C2H4), ethane (C2H6), propylene (C3H6), propane (C3H8), and 1-butene (C4H8), among&nbsp;others.&nbsp;The <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=990+micro">Agilent 990 Micro GC</a> enables fast and accurate detection of ethylene or propylene stream cracking gas products, a fundamental measure for determining the effectiveness of the cracking process. The system's demonstrated utility in refinery gas analysis further supports its suitability.<h4>Conclusion&nbsp;</h4>This study demonstrates the applicability of the Agilent 990 Micro GC for analyzing ethylene or propylene stream cracking gas products, providing essential process control data for optimizing cracking production and yield. Quantitation precision was evaluated through 10&nbsp;consecutive analyses of calibration standard gases, showing retention time (RT) repeatability (%RSD) less than 0.1% and area repeatability (%RSD) less than 1.0% for all compounds. These results confirm the instrument's excellent performance in reliably qualifying and quantifying these stream cracking gas&nbsp;products.<h3>2. EST Analytical: Purge and Trap Extraction of Tea Flavor Components</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_Tea_Flavor_Analysis_by_Purge_and_Trap_9bb392c2c1.pdf">Full PDF for download</a></li></ul>Purge and Trap (P&amp;T) sampling is a universally accepted technique for the analysis of volatile compounds in water. The United States Environmental Protection Agency (USEPA), the World Health Organization (WHO) and the American Society for Testing and Materials (ASTM) have all published methods using P&amp;T for water matrices. However, food and flavor manufacturers have yet to use this technique for the analysis of the volatile flavor components of their products. SPME has become the more accepted technique for flavor analysis.&nbsp;Both SPME and P&amp;T have their limitations. P&amp;T is recommended for volatile analytes and does not work when compounds have higher boiling points. Still, P&amp;T is a reliable technique that has the ability to purge out all of the volatile analytes of a system and detect very low concentrations of those analytes. On the other hand, SPME can be used for sampling a larger amount of semi-volatile compounds and fiber coating selection aids in better discrimination of analyte sampling. Yet, SPME is not an exhaustive sampling technique thus there are detection limitations to the technique. This application note will examine the analysis of white tea samples using P&amp;T sampling.&nbsp;<h4>Experimental</h4>The <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/2160">EST Analytical Evolution Purge and Trap</a> was set up with a Vocarb™ 3000 trap while the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/2159">Centurion WS autosampler </a>was set to run in soil mode. The sampling system was configured to an <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=7890">Agilent 7890A Gas Chromatograph (GC) </a>and <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=5975C">5975C inert XL Mass Spectrometer (MS) </a>for separation and analysis. As the compounds of interest for this analysis were volatile, a Restek Rxi® 624 Sil MS 30m X 0.25mm X 1.8um column was affixed in the GC. Sampling and analysis parameters were optimized and are listed in Tables 1 and 2.<h4>Conclusions</h4>Using purge and trap to evaluate the flavor compounds of the tea samples was a reliable sampling technique. The findings were repeatable and the chromatography was excellent. The resulting flavor compounds were easily purged out of the tea matrix and as the technique is exhaustive, there was excellent detection of the flavor compounds in the system. This sampling technique established purge and trap to be an exceptional method for the determination of volatile analytes in tea.<h3>3. Shimadzu: Real-Time Measurement of CH4 and CO2 Concentrations for Estimating Methane Emissions from Rice Fields</h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_01_00887_en_adf24e951d.pdf">Full PDF for download</a></li></ul><h5>User Benefits</h5><ul><li>The portability of this gas analyzer means the user can decide where to place it, such as near a rice field, to continuously measure CH4 and CO2 emissions.&nbsp;</li><li>The CGT-7100 analyzer unit has a built-in pump, filter, dehumidifier, and other sample pretreatment equipment, so it does not require other equipment to perform measurements.</li><li>Data can be stored on a USB flash drive for easy editing on a computer or sharing with other departments.</li></ul>CH4 is a gas that has a greenhouse effect about 28 times greater*1 than CO2. One source of CH4 gas emissions is flooded rice fields. They release the CH4 gases generated by microorganisms living in the soil into the atmosphere. Since CH4 emissions from rice fields account for a significant proportion of greenhouse gases emitted from the agriculture, forestry, and fishery industry, various measures are being implemented to reduce emissions, such as managing the water and soil used in rice fields and improvingthe fertilizers used.&nbsp;The closed chamber method measures variations in gas concentrations due to gases exchanged with plants, such as rice. 1) In this article, a <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=1&amp;search=CGT-7100">CGT-7100</a> portable gas analyzer measures the concentration of CH4 and CO2 generated inside a specialized chamber placed on the surface of rice paddy soil.<h4>CH4 Emitted from Rice Fields&nbsp;</h4>The amount of CO2 emitted from a rice field depends on the amount breathed (emitted) from the rice plant and photosynthesized (absorbed), whereas the amount of CH4 emitted depends on the microorganisms in the soil. Fig. 2 illustrates the process of CH4 emission from rice fields. The microorganisms generate CH4 by decomposing organic matter in the soil. When a rice field is flooded with water, the supply of oxygen to the soil stops and anaerobic microorganisms actively generate CH4. It is thought that the generated CH4 is emitted into the atmosphere via two pathways. One pathway is via the roots and stalks of the rice plants (pathway 1).2),3) Due to the functions of the microorganisms, CH4 concentrations in the soil become higher than inside the plant, resulting in a concentration gradient that dissolves into the root cells. The dissolved CH4 becomes a gas within the narrow gaps between cells and moves along the gaps to the leaf sheath above ground. Pores on the leaf surface then discharge the CH4 into the atmosphere. In the other pathway (pathway 2), CH4 in the soil forms bubbles that are released directly into the atmosphere without passing through the rice plant. Pathway 1 increases the CH4 concentration inside the chamber by a certain proportion, but the quantity and frequency of CH4 emissions via pathway 2 are not clearly known, so there is an element of uncertainty about the estimated quantity of CH4 emitted from rice fields4). Therefore, the frequency that bubbles formed was estimated by analyzing the CH4 concentration measurement results to determine how quickly the CH4 concentration increasedper unit area (methane flux).<h4><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=1&amp;search=CGT-7100">CGT-7100 Portable Gas Analyzer&nbsp;</a></h4>The CGT-7100 is an all-in-one portable continuous gas concentration measuring system (Fig. 3). Because the compact main unit includes a pretreatment unit with a built-in electronic cooler for removing water moisture, a filter for removing dust, and a pump for suctioning sample gas into the analyzer system, the analyzer can be operated independently*2. Up to three components can be selected for measurement. In addition to two of the CO2, CO, and CH4 components being measured by the non-dispersive infrared absorption (NDIR) method, one component can also be selected for measurement by an O2 analyzer (optional), based on the limiting current type zirconia method. Changes in concentrations over time can be monitored with a wide range of measurements, from ppm to vol%. With the minimum sample gas flowrate of 100 mL/min (optional), gas concentrations can be measured in small sample quantities, and the sample gas flowrate can be varied within the range of 100 to 400 mL/min. As shown in the measurement process flow diagram below, samples can also be measured without losses by including a recirculation system that returns the sample gas discharged from the analyzer to the measurementlocation (inside the chamberin this case).<h4>Non-Dispersive Infrared Absorption (NDIR) Method&nbsp;</h4>The CGT-7100 uses the non-dispersive infrared absorption (NDIR) method for measurements. CO2 and other heteronuclear gases have unique infrared light absorption spectra. Gas concentrations can be measured selectively by passing infrared light through the sample gas and using the detector to measure the quantity of infrared light in the absorption band that is unique to a given type of gas. Robust and reliable measurements are achieved with the optical system in the NDIR unit, which has an excellent track record among online gas analyzers.<h4>Conclusion&nbsp;</h4>This article describes an example of using a CGT-7100 portable gas analyzer to estimate the amount of CH4 and CO2 emitted from a rice field by continuously measuring CH4 and CO2 concentrationsinside the chamberplaced in a rice paddy.&nbsp;Since the CGT-7100 is a continuous gas analyzer, it is ideal for measuringchangesin gas concentrationsin realtime. The CGT-7100 can be used to observe changes in the levels of CH4 and CO2 or the effects of bubble formation when implementing rice field water and soil management or fertilizer improvement measures.&nbsp;With its built-in sample gas pretreatment and sampling functionality, gas concentrations can be conveniently measured without the need for additional equipment, and the portability of the analyzer means it can measure gas concentrations in a wide variety of locations. If used with a communication unit, measurement data can be viewed and saved remotely via a computer or tablet to accommodate a wide range of testing and research applications.

News from LabRulezGCMS Library - Week 52, 2025

Our Library never stops expanding. What are the most recent contributions to LabRulezGCMS Library in the week of 29th December 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 Shimadzu!<h3>1. Agilent Technologies: Fatty Acid Methyl Ester Analysis Using the Agilent 8850 GC System</h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_fame_analysis_8850_gc_5994_8743en_agilent_2bed33b70d.pdf">Full PDF for download</a></li></ul>Fatty acids are components of fat and are an essential component of a healthy diet. They are found in a variety of foods, including oily fish, nuts, seeds, and vegetable oils. Fatty acids can be categorized as saturated fat, monounsaturated fat, polyunsaturated fat (including omega-3 and omega-6 fatty acids), and trans fat. Unsaturated fatty acids play a beneficial role in maintaining heart and vascular performance. However, artificial trans fatty acids, found in processed foods, should be strictly limited. The measurement of fatty acids in food plays an important role in:<ul><li>Nutritional assessment: Analyzing the omega-3/omega-6 ratio for dietary nutrient balance&nbsp;</li><li>Safety regulation: Identifying health risks such as trans fatty acids&nbsp;</li><li>Quality control: Detecting oil adulteration and process&nbsp;defects&nbsp;</li><li>R&amp;D support: Providing data support for the development of functional foods&nbsp;</li></ul>Techniques available for fatty acid determination in food include gas chromatography, liquid chromatography, and spectroscopic techniques. Each technique has its own advantages, disadvantages, and applicable scenarios. For example, liquid chromatography is suitable for analyzing heat-labile fatty acids, but it suffers from low resolution. Fluorescence spectroscopy is simple to operate but susceptible to matrix effects and poor specificity. Gas chromatography is the most used technique for fatty acid measurement. Fatty acids in food primarily exist in the form of triglycerides. Before analysis, triglycerides must be extracted, saponified, and methylated to the corresponding FAMEs. FAMEs are less polar and more volatile than fatty acids, making them suitable for analysis on gas chromatography platforms. Polar columns, such as those with polyethylene glycol and cyanopropyl siloxane stationary phases, are primarily used for the FAMEs analysis. Polyethylene glycol stationary phases are good at analyzing simple fatty acid mixtures and are not suitable for the analysis of cis-trans isomers. A column coated with high‑content cyanopropyl phase is recommended in different analytical methods for FAMEs analysis. However, an analysis based on this phase type usually takes more than 70 minutes to finish, and the retention time (RT) stability is not very good. The Agilent J&amp;W DB-FastFAME column features a modified cyanopropyl phase to accelerate the analysis and improve&nbsp;repeatability.&nbsp;Agilent offers DB-FastFAME columns in different dimensions; the 20-meter and 30-meter sizes can help improve the analysis speed for 37 representative FAMEs in food. Previous work demonstrated the analysis speed improvement using the conventional oven ramp rate on the two columns.1 With the launch of the Agilent 8850 GC, rapid temperature programming can be achieved in an air bath oven. This application note demonstrates the fast analysis of 37 FAMEs using nitrogen (N2 ) and helium (He) carrier gases on the 8850&nbsp;GC. Meanwhile, more complex FAME mixtures including 37&nbsp;FAMEs and 15 trans FAMEs were analyzed on a 90-meter DB-FastFAME column and a 100-meter Agilent J&amp;W HP-88 column to demonstrate the 8850 GC performance in cis/trans FAMEs and position isomers analysis.<h4>Experimental</h4><h5>Instrumentation&nbsp;</h5>An <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=8850+GC">8850 GC system </a>equipped with a split/splitless inlet and a flame ionization detector (FID) was used for the analysis. An <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=7650A">Agilent 7650A automatic liquid sampler (ALS)</a> (part&nbsp;number&nbsp;G4567A) was applied for sample injection.&nbsp;The methods performed on the four analytical columns using He and N2 carrier gases are listed in Table 1. The settings on inlet and detector temperatures are the same. The column head pressure and the oven temperature program were optimized based on the column type and carrier gas. Data were acquired and processed using <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=OpenLab+CDS">Agilent OpenLab CDS</a> 2.8. The list of consumables used is shown in Table 2.<h4>Results and discussion&nbsp;</h4><h5>Fast analysis of 37 fatty acid methyl esters on short&nbsp;columns&nbsp;</h5>The 37 FAMEs mimic the fatty acid composition of many food samples, including most of the important saturated, monounsaturated, and polyunsaturated FAMEs. They are well‑established and widely accepted reference materials.&nbsp;A 20 m × 0.18 mm&nbsp;id, 0.2&nbsp;µm DB-FastFAME&nbsp;column and a 30&nbsp;m × 0.25 mm&nbsp;id, 0.25 µm DB-FastFAME&nbsp;column were used to demonstrate the high-speed analysis of 37 FAMEs on the 8850 GC. The oven ramp program and column flow rate were based on previous work and further optimized for the 8850 GC. Both He and N2 carrier gas-based methods were developed considering the increasing alternative carrier gas need and lab operation habits in different regions.&nbsp;The GC-FID chromatograms obtained on the two columns using different carrier gases are shown in Figures 1A, 1B, 2A, and 2B. All compounds were well resolved in the He methods. Three compound pairs that cannot be baseline-separated are shown in black squares. Among them, the peaks of c22:2n6 and c23:0 had the lowest resolution of 1.27 and 1.31 on the 20-meter and 30-meter columns, respectively, using the He method. The AOAC International Method 996.062 requires separating the FAME pair of adjacent peaks of C18:3 and C20:1 and the FAME trio of adjacent peaks of C22:1, C20:3, and C20:4 with a resolution of 1.0 or greater. This requirement is mainly recommended for high-content cyanopropyl 4 stationary phases. The six probe FAMEs eluted in different orders on the DB-FastFAME column, as marked by the yellow squares in the chromatogram. Their separation exceeded the resolution requirement easily due to the DB-FastFAME column's unique selectivity. The analysis times of the He methods were less than 7 minutes and 10 minutes on the two columns. The analysis speed was five to eight times faster than that of conventional methods.<h4>Conclusion&nbsp;</h4>A high-speed FAMEs analysis was achieved on an Agilent&nbsp;8850 GC system with excellent repeatability when running the FAMEs standards on specially engineered 20-meter and 30-meter Agilent J&amp;W DB-FastFAME columns under optimized oven programs. The analysis time is less than 10&nbsp;minutes using He carrier gas and less than 15&nbsp;minutes using N2 carrier gas, which is five to eight times faster than the conventional method. Peak resolutions obtained by the fast methods met the AOAC 996.06 standard requirements. The methods can help improve lab productivity significantly for routine analysis of 37 FAMEs.&nbsp;The analysis of 52 FAMEs on 90-meter DB-FastFAME and 100-meter Agilent J&amp;W HP-88 columns demonstrated that the 8850 GC can deliver performance equivalent to the Agilent 8890 GC system when analyzing complex fatty acids—including cis/trans fatty acids and positional isomers— in terms of resolution, area repeatability (&lt; 2.5%), and RT&nbsp;precision (&lt; 0.04%).<h3>2. Shimadzu: Quantification of 8 Disinfection Byproducts from Water by Liquid-Liquid Extraction and Gas Chromatography-MassSpectrometry</h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_07_2507_en_52b8f30f0c.pdf">Full PDF for download</a></li></ul>Disinfectants such as chlorine and chloramine are widely used to eliminate microorganisms in water. However, these disinfectants react with naturally occurring chemical constituents, such as amino acids and other labile organic chemicals, forming a range of disinfection byproducts (DBPs). Chronic exposure to DBPs elevates the risk of developing cancer, liver damage, and decreased nervous system activity. Hence, accurate detection and quantification of DBPs in water is crucial.&nbsp;Although official recommended method for measuring DBPs is based on GC/ECD, GC/MS offers significant advantages in terms of simultaneous quantification and identification of both known and unknown compounds in a single analysis, providing comprehensive data on complex water samples. Unlike ECD, which has a limited dynamic range and can only detect electroactive compounds, MS offers a broader dynamic range, allowing the detection of analytes at varying concentrations. Additionally, GC/MS provides superior sensitivity, specificity, and structural information, making it the ideal method for detailed, high-precision analysis of disinfection byproducts and other water contaminants.<h4>2.2. Analytical Conditions</h4><h5>Preparation of instrument and analysis:</h5>The analytical method was established, and the instrument parameters are detailed in Table 1. Prior to the analysis, both the instrument and the column were conditioned. The “HighSensitivity” autotune mode of the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=1&amp;search=GCMS-QP2020+NX">GCMS-QP2020 NX</a> was used for the analysis. A standard solution containing 500 ppb of the target analytes, surrogate, and internal standard was injected using the MS fullscan mode to determine the retention times.The peaks corresponding to the target compounds, internal standard, and surrogate were identified using the NIST GC/MS library. Quantifier and qualifier ions for each analyte were selected, and a compound table was created accordingly and the same was used to develop a Scan/SIM method using the “Creation of Automatic Scan/SIM Table” (COAST) wizard within the GCMSsolutionTM software. The ultra-fast scanning capability (20,000 u/s) of the GCMS-QP2020 NX enables simultaneous acquisition of Scan and SIM events without compromising data quality.&nbsp;The newly created Scan/SIM method was used for the quantification and reporting of analytical data. Calibration standards were analyzed. The data and the calibration curve, using the internal standard method, were processed using LabSolutions InsightTM software which enables the analysis of large numbers of data simultaneously. Following this, both the unspiked and spiked (5 ppb) samples were analyzed and quantified.<h4>3. Result and Discussion</h4>A 6-point calibration curve was created for all target analytes. A good linear response, with correlation coefficients (r²) greater than 0.99, and accuracy within 80-120% was observed for all analytes. A signal-to-noise ratio (S/N) ≥ 10 was observed for all analytes at 5 ppb standard. The results are shown in Table 2.<h4>4. Conclusion</h4><ul><li>A highly sensitive GC/MS method was developed for 8 halogenated DBPs using Shimadzu GCMS-QP2020 NX following USEPA 551.1 sample preparation protocol.&nbsp;</li><li>Excellent linearity results and recovery results at 5.0 ppb concentration for all the analytes demonstrate that the analytical workflow is suitable for analyzing the listed DBPs in tap water using GC/MS technique at a low concentration level.</li></ul>

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