<p><strong>In this troubleshooting tip, Genevie Hodson, Senior Manager of Technical Support and Applications at Phenomenex, addresses a common solid phase extraction (SPE) question:</strong></p><blockquote><p><strong>"My sample won't flow through my SPE cartridge. Why is this happening?"</strong></p></blockquote><p>Several factors can contribute to flow problems during SPE. A systematic troubleshooting approach can help identify the root cause and restore proper cartridge performance.</p><h3><strong>Identifying When the Flow Problem Occurs</strong></h3><p>The first step in troubleshooting is determining <strong>when</strong> the flow issue appears.</p><p>Ask the following question:</p><ul><li>Does the problem occur during the <strong>sample loading step</strong>?</li><li>Or does it occur <strong>before sample loading</strong>, during cartridge conditioning or when running blanks?</li></ul><p>The timing of the problem can help identify its underlying cause.</p><h3><strong>Cause 1: Viscous or Cloudy Samples</strong></h3><h4><strong>Description</strong></h4><p>Samples that are thick, highly viscous, or contain large amounts of particulate matter can restrict flow through the SPE sorbent.</p><h4><strong>Recommended Actions</strong></h4><p>Before SPE, the sample should be:</p><ul><li>Diluted</li><li>Centrifuged</li><li>Filtered</li></ul><p>Another option is selecting a sorbent with a larger particle size.</p><h4><strong>Example</strong></h4><ul><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products?category=6&amp;manufacturerItems=50&amp;search=x"><strong>Strata-X</strong></a> – 33 µm particle size</li><li><strong>Strata XL</strong> – 100 µm particle size</li></ul><p>The larger particle size of Strata XL is better suited for viscous samples and can improve flow performance.</p><h4><strong>When This Problem Appears</strong></h4><p>If sample viscosity or particulate content is the cause, the flow issue will typically occur during the <strong>sample loading step</strong>.</p><h3><strong>Cause 2: Insufficient Manifold Pressure</strong></h3><h4><strong>Description</strong></h4><ul><li>Flow problems may originate from the SPE manifold or instrumentation.</li><li>The applied pressure must be sufficient to generate proper flow through the cartridge.</li></ul><h4><strong>Recommended Actions</strong></h4><p>Check:</p><ul><li>The SPE manifold</li><li>Associated instrumentation</li><li>Individual manifold positions</li></ul><p>In some cases, a specific position within the manifold may be responsible for the problem.</p><h4><strong>When This Problem Appears</strong></h4><p>If manifold pressure is the issue, poor flow will typically be observed during:</p><ul><li>Conditioning steps</li><li>Blank runs</li></ul><h3><strong>Cause 3: Immiscible Solvents</strong></h3><h4><strong>Description</strong></h4><p>Using solvents that are not mutually miscible can interfere with flow through the SPE cartridge.</p><h4><strong>Recommended Actions</strong></h4><p>Always use solvents that are miscible with each other.</p><h4><strong>Example</strong></h4><ul><li>Hexane</li><li>Water</li></ul><p>These solvents are immiscible and may cause flow problems if used together.</p><h4><strong>When This Problem Appears</strong></h4><p>Flow issues caused by solvent incompatibility are generally observed during:</p><ul><li>Conditioning steps</li><li>Blank runs</li></ul><h3><strong>Cause 4: Precipitation and Protein Build-Up</strong></h3><h4><strong>Description</strong></h4><ul><li>Sample constituents or proteins may precipitate and clog the sorbent bed.</li><li>This blockage can significantly restrict or stop flow through the cartridge.</li></ul><h4><strong>Recommended Actions</strong></h4><p>Possible corrective actions include:</p><ul><li>Diluting the sample</li><li>Reducing sample volume</li><li>Avoiding denaturing solvents</li><li>Washing the sorbent with a low ionic strength buffer before the regular wash step</li></ul><h4><strong>When This Problem Appears</strong></h4><p>If protein precipitation or sample-derived precipitates are responsible, the flow problem will typically occur <strong>after the sample has been loaded</strong>.</p><h3><strong>Systematic Troubleshooting Approach</strong></h3><p>When investigating SPE flow issues, use a systematic elimination strategy.</p><h3><strong>Key Principle</strong></h3><ul><li>Evaluate one variable at a time and isolate potential causes individually.</li><li>This approach helps identify the true root cause rather than changing multiple parameters simultaneously.</li></ul><h3><strong>Summary of Common SPE Flow Problems</strong></h3><h5><strong>Cause &nbsp; / &nbsp; Typical Observation Point &nbsp; / &nbsp; Suggested Solution</strong></h5><ul><li><strong>Viscous or cloudy sample: </strong>During sample loading - Dilute, centrifuge, filter, or use larger particle size sorbent</li><li><strong>Insufficient manifold pressure: </strong>Conditioning or blanks - Check manifold and instrumentation</li><li><strong>Immiscible solvents:</strong> Conditioning or blanks - Use only miscible solvents</li><li><strong>Precipitation or proteins: </strong>After sample loading - Dilute sample, reduce volume, avoid denaturing solvents, use low ionic strength buffer wash</li></ul><h3><strong>Conclusion</strong></h3><p>Flow problems in SPE can arise from several common sources, including viscous samples, insufficient manifold pressure, incompatible solvents, and precipitation of sample components or proteins. Determining exactly when the problem occurs during the SPE workflow is a critical first step in troubleshooting. A systematic, one-variable-at-a-time approach allows the root cause to be identified efficiently and corrective actions to be implemented.</p>

SPE Troubleshooting: Why Won't My Sample Flow Through the SPE Cartridge?

<p><span><strong>Time is running out to take advantage of discounted registration fees for the 19th Czech-Slovak Spectroscopic Conference (19th CSSC), one of the leading scientific events dedicated to spectroscopy and spectrometry in Central Europe. Researchers, students, instrument specialists, and industry professionals are invited to join the conference at the Faculty of Science, Palacký University Olomouc. The Early Bird registration period and the deadline for lecture and poster abstract submission both end on June 15, 2026.&nbsp;</strong></span></p><h3><strong>Registration</strong></h3><blockquote><p class="cke-user_style-important"><strong>👉</strong><a target="_blank" rel="noopener noreferrer" href="https://cssc2026.spektroskopie.cz/registration_online"><strong>Online registration form</strong></a></p></blockquote><h4><strong>Registration Fees</strong></h4><h5><strong>Early (before June 15, 2026)</strong></h5><ul><li><strong>Participant (Member of IMMSS and SSS): </strong>10 000 CZK&nbsp;&nbsp;</li><li><strong>Participant (Non-member of IMMSS and SSS): </strong>14 000 CZK&nbsp;&nbsp;&nbsp;</li><li><strong>Students: </strong>7 000 CZK&nbsp;</li><li><strong>1-day registration:</strong> 5 000 CZK</li><li><strong>Accompanying person*: </strong>5 000 CZK</li></ul><h5><strong>Regular (after June 15, 2026)</strong></h5><ul><li><strong>Participant (Member of IMMSS and SSS): </strong>13 000 CZK&nbsp;&nbsp;</li><li><strong>Participant (Non-member of IMMSS and SSS): </strong>18 200 CZK&nbsp;&nbsp;&nbsp;</li><li><strong>Students: </strong>9 100 CZK&nbsp;</li><li><strong>1-day registration:</strong> 6 500 CZK</li><li><strong>Accompanying person*: </strong>6 500 CZK</li></ul><p><i>* The accompanying person does not have access to the scientific programme</i></p><p><strong>The conference fee is calculated with VAT</strong> and includes:</p><ul><li>attendance to lectures and poster session</li><li>book of abstracts (electronic version)</li><li>booklet</li><li>lunches, refreshments (coffee/tea breaks)</li><li>excursion</li><li>attendance at Welcome Party and Gala Dinner.&nbsp;</li></ul><p><strong>For an accompanying person</strong>, the conference fee includes the Welcome Party, the excursion and the Conference Dinner. The Conference Dinner is not included in the 1-day registration. This payment should be arranged with the Organising Committee.</p><p><i><strong>Accommodation is not included in the conference fee.</strong></i></p><h3><strong>Abstract submission</strong></h3><blockquote><p class="cke-user_style-important"><strong>👉</strong><a target="_blank" rel="noopener noreferrer" href="https://cssc2026.spektroskopie.cz/abstract_submission_online"><i><strong>ABSTRACT SUBMISSION FORM</strong></i></a></p><p><strong>Deadline</strong> for lecture/poster abstract submission <strong>is June 15, 2026</strong></p></blockquote><h4><strong>Posters</strong></h4><p>Prepare your poster in<strong> English in the format A0</strong> vertically orientated (portrait). The presence of one of the authors at the poster is requested during the poster session. Materials for mounting posters will be available on the poster panels.</p><h4><strong>Lectures</strong></h4><p>Prepare your <strong>presentation in English</strong> in <strong>PowerPoint</strong> of Portable Document Format (<strong>pdf</strong>), both in format <strong>16:9</strong> (widescreen). <strong>Invited and oral lectures</strong> takes <strong>30</strong> and<strong> 20 minutes </strong>(including discussion), respectively.&nbsp;</p><h3><strong>TOPICS &nbsp; &nbsp; &nbsp; &nbsp; &nbsp; &nbsp; &nbsp; &nbsp; &nbsp; &nbsp;&nbsp;</strong></h3><h4><strong>Czech - Slovak Spectroscopic Conference</strong></h4><ul><li>Atomic spectrometry (AAS, ICP-MS, AFS, OES, speciation analysis, etc.)</li><li>Molecular spectrometry/spectroscopy (UV-Vis, NMR, IR, Raman, circular dichroism, etc.)</li><li>New techniques and data processing methods in IR and Raman spectroscopy, Special methods of Raman spectroscopy (resonance Raman, SERS, SERRS, TERS)</li><li>XRF spectrometry (EDS, WDS, XRF, PIXE, etc.)</li><li>Mass spectrometry &amp; hyphenated techniques</li><li>Instrumental radioanalytical methods (Gamma spectroscopy, NAA, etc.)</li><li>Laser spectroscopy and special spectroscopy techniques</li><li>Sample preparation and introduction techniques</li><li>Applications &nbsp;of atomic and molecular spectroscopy</li><li>Statistics and metrology in spectroscopy</li></ul><h4><strong>Mössbauer Spectroscopy in Material Science</strong></h4><ul><li>Environmental, catalytic, biologic, medical applications</li><li>Magnetism, magnetic nanoparticles, molecular magnets</li><li>Nanomaterials, nanostructures, nanocomposites, core-shell nanoparticles, thin films</li><li>Nanomaterials in biomedicine</li><li>Nuclear forward scattering in materials science</li><li>Solid-state chemistry and physics</li><li>Industrial applications, corrosion</li><li>Instrumentation, software</li><li>Earth Science, Mineralogy and Archaeology</li></ul><h4><strong>Venue</strong></h4><h5><strong>Faculty of Science</strong></h5><ul><li>Palacky University Olomouc</li><li>17. listopadu 1192/12, &nbsp;Olomouc, Czech Republic</li></ul>

19th CSSC 2026: Early Bird Registration and Abstract Submission Deadline Approaching

<p><strong>Our Library never stops expanding. What are the most recent contributions to LabRulezGCMS Library in the week of 8th June 2026? Check out new documents from the field of the gas phase, especially GC and GC/MS techniques!</strong></p><blockquote><p><span style="font-size:20px;">👉 </span><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library"><span style="font-size:20px;"><strong>SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT GCMS AND RELATED TECHNIQUES</strong></span></a></p></blockquote><blockquote><p><strong>👉 Need info about different analytical techniques?</strong> Peek into <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library"><strong>LabRulezLCMS</strong></a> or <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library"><strong>LabRulezICPMS</strong></a> libraries.</p></blockquote><p>This week we bring you application notes by <strong>Agilent Technologies </strong>and<strong> Shimadzu</strong>, poster by <strong>MDCW / William &amp; Mary </strong>and brochure by<strong> Thermo Fisher Scientific!</strong></p><h3><strong>1. Agilent Technologies: Analysis of Bisphenol A in PET Granules Using the </strong><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=8890"><strong>Agilent 8890</strong></a><strong>/</strong><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=5977C"><strong>5977C</strong></a><strong> GC/MS System</strong></h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_bisphenol_a_pet_granules_gc_ms_system_5994_9240en_agilent_b9b78ea413.pdf"><strong>Full PDF for download</strong></a></li></ul><section><div><div><div><div><div><div><p>Polyethylene terephthalate (PET) is commonly used in the food and beverage industry, as it is easy to recycle. Contaminants in recycled PET, including acetaldehyde, benzene, limonene, and bisphenol A (BPA), can migrate from the packaging into the contents, potentially affecting the safety and quality of the products stored inside.<sup>1</sup> Monitoring these contaminants is crucial for ensuring the quality of recycled PET products, as they can affect the physical, chemical, and sensory properties of recycled PET, potentially leading to product defects or health concerns.<sup>1</sup> FSSAI officially permits the use of recycled PET (rPET) in food packaging, subject to strict safety and quality standards. This regulatory change was formalized through amendments notified in March 2025, effective immediately.<sup>2</sup> All recycled plastics used in food contact applications must comply with stringent overall and specific migration limits to ensure no harmful chemical transfer into food. The recycling processes require validated decontamination steps to reduce contaminants to safe levels. Manufacturers must certify their packaging materials under FSSAI guidelines.&nbsp;</p><p>GC/MS plays a critical role in assessing the safety and suitability of recycled plastics for food‑contact applications. The method adopted in this work demonstrates the use of an Agilent 8890 GC system coupled with an <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=5977C"><strong>Agilent 5977C GC/MS system</strong></a> for quantification of BPA in PET granules.</p><h4><strong>Conclusion&nbsp;</strong></h4><p>This application note presents key strategies for the analysis of BPA in PET granules using GC/MS. The calibration used here ranged from 10 to 500 ng/mL, and the LOQ of the method was demonstrated at 500 ng/g for a PET sample. Repeatable results were found for six successive replicates of matrix-based standards at 100 ng/mL. Satisfactory recoveries were obtained for the tested matrix at 500 ng/g spiked concentration levels. Thus, this study demonstrates the applicability of this method for routine analysis of PET samples for identification and quantification of BPA.</p><h3><strong>2. MDCW / William &amp; Mary: Characterizing PqsE’s enzymatic activity in Pseudomonas aeruginosa by Volatile Organic Compound analysis with GC×GC-TOFMS</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/Zimmermann_Nicolas_a9c80563a3.pdf"><strong>Full PDF for download</strong></a></li></ul><section><div><div><div><div><div><div><p>Pseudomonas aeruginosa is an opportunistic pathogen commonly associated with severe respiratory infections in immunocompromised patients. The pathogenic behaviors of P. aeruginosa are controlled by a cell-to-cell communication system called quorum sensing (QS). Many genes activated by QS include those responsible for forming biofilms and producing virulence factors. Interestingly, several virulence factors produced by P. aeruginosa are regulated by an interaction between a receptor, RhlR and a hydrolase, PqsE. Thus, the PqsE-RhlR interaction has become a target for antibiotic development and further characterization. Comprehensive two-dimensional gas chromatography paired with time-of-flight mass spectrometry (GC×GC-TOFMS) was chosen for metabolomic analysis as it is known for its high sensitivity and improved peak capacity. With GC×GC-TOFMS, the volatile organic compound (VOC), acetophenone, was discovered and utilized to measure dose-dependent inhibition of PqsE’s enzymatic activity in vivo by the small molecule inhibitor, Vorinostat. Furthermore, additional VOCs were identified that could add additional insight to PqsE’s function.</p><h4><strong>Experimental:</strong></h4><ul><li><strong>GC/MS:</strong> <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/1097"><strong>Pegasus BTX (LECO)</strong></a> with <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/82"><strong>LECO L-PAL3 Autosampler</strong></a></li><li><strong>Software:</strong> <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/348"><strong>ChromaTOF Tile</strong></a></li></ul><h4><strong>Summary</strong></h4><p>Eight VOCs identified that show statistically significant concentration differences between WT and D73A samples. The VOC acetophenone can be used to measure the enzymatic inhibition of PqsE in vivo. Vorinostat displayed a dose-dependent decrease in acetophenone levels.</p><h3><strong>3. Shimadzu: Extractable Study of Container Closure Pack Used to Store Oral Drug Product Using Dynamic Headspace Technique</strong></h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_06_sip_gc_044_en_ef833b01f0.pdf"><strong>Full PDF for download</strong></a></li></ul><h5><strong>User Benefits</strong></h5><ul><li>ASSP and simultaneous Scan/MRM analysis facilitating accurate qualitative identification and quantitation at the same time.</li><li>Dynamic headspace enables concentrating the analytes in cold trap with multi-injection count and helps to achieve higher sensitivity overstatic headspace, especially for trace level quantitation.</li></ul><p>Extractable and leachable (E &amp; L) studies are becoming increasingly important in the pharmaceutical industry as it is a mandatory requirement from FDA during filing of the drug product. The purpose of E &amp; L studies is to identify and evaluate possible toxicological risks. In this study, the regulatory references aim to identify traces of potential chemical substances. These substances may be harmful to patients due to their toxicity or may impact the activity of the drug product. Hence, to ensure the safety and efficacy of the drug throughout itsshelf-life, E &amp; L studies play an important role.&nbsp;</p><h5><strong>What Are Extractables and Leachables?&nbsp;</strong></h5><p>Extractables are organic and inorganic chemical entities that are released from a pharmaceutical packaging/delivery system, packaging component, or packaging material of construction into an extraction solvent under laboratory conditions[1].&nbsp;</p><p>Leachables are foreign organic and inorganic chemical entities that are present in a packaged drug product because they have leached into the packaged drug product from a packaging/delivery system, packaging component, or packaging material of construction under normal conditions of storage and use or during accelerated drug product stability studies[1].</p><h4><strong>Methods of Analysis</strong></h4><p>In this method, fifteen standards were analyzed by <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=1&amp;search=GCMSTQ8050+NX"><strong>GCMSTQ8050 NX</strong></a> with <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=1&amp;search=HS-20+NX"><strong>HS-20 NX</strong></a> (Trap) autosampler. For the method suitability, several important parameters like system suitability, linearity and precision were performed.&nbsp;</p><h4><strong>Conclusion</strong>&nbsp;</h4><p>The chromatographic profile of solvent reflux experiment shows higher number of extractables than aqueous incubation. Furthermore, in aqueous incubation, the content of extractables is well below the AET level. Since, placebo of the ophthalmic drug product is completely aqueous, CCP used in the analysis is totally safe and can be used for the storage of Penicillin V.&nbsp;</p><p>Shimadzu’s GCMS-TQ provides high scan speed of 20000 amu/sec with ASSP technology enabling simultaneous SCAN/MRM analysis which is crucial in E&amp;L study.&nbsp;</p><p>Generally, if the drug product falls under parenteral and oral drug product (PODP), evaluation threshold will be at higher side due to having wider SCT. However, AET for Penicillin V was at too low to evaluate with liquid injection and static headspace technique. This has been proved with the trap headspace technology.&nbsp;</p><p>To analyze the complete extractable profile with the sample screening is only possible with dynamic headspace as most of the extractables were not detected in the injection acquired with static headspace.</p><h3><strong>4. Thermo Fisher Scientific: </strong><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/2419"><strong>Thermo Scientific™ Orbitrap Exploris™ GC S Mass Spectrometer</strong></a></h3><ul><li>Brochure</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/br_004035_gc_orbitrap_exploris_gc_s_enviro_br004035_na_en_b1fad7f3af.pdf"><strong>Full PDF for download</strong></a></li></ul><p>The <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/2419"><strong>Thermo Scientific Orbitrap Exploris GC S</strong></a> is a high-resolution GC-MS system designed specifically for environmental and food safety laboratories performing analysis of persistent organic pollutants (POPs). Combining Orbitrap high-resolution accurate-mass (HRAM) technology with the proven Advanced Electron Ionization (AEI) source, the platform delivers exceptional sensitivity, selectivity, and robustness for demanding applications such as dioxins, dioxin-like PCBs, PFAS, pesticides, and emerging contaminants. The system is engineered to meet regulatory requirements while supporting multiple analytical workflows on a single instrument.</p><p>For dioxin and POPs analysis, the Orbitrap Exploris GC S offers performance traditionally associated with high-resolution magnetic sector instruments while providing a more streamlined and user-friendly workflow. The instrument achieves ultra-trace sensitivity, excellent repeatability, and regulatory-compliant mass resolution, supported by dedicated solutions including the TRACE Dioxin column, <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/422"><strong>TriPlus RSH SMART</strong></a> autosampler, and Chromeleon Dioxin HRAM eWorkflow software. Automated method templates, built-in quality control checks, and compliance-ready reporting simplify implementation and routine operation, enabling laboratories to increase throughput while maintaining confidence in analytical results.</p><p>The platform also excels in pesticide screening and quantitation across complex food and environmental matrices. High-resolution full-scan acquisition, wide dynamic range, accurate-mass measurements, isotope pattern confirmation, and extensive spectral library matching allow confident identification and quantitation of hundreds of compounds in a single analysis. The ability to perform retrospective data analysis enables laboratories to answer new regulatory or research questions without reinjecting samples, providing flexibility for evolving analytical requirements.</p><p>Supporting the mass spectrometer is a complete analytical ecosystem that includes Chromeleon Chromatography Data System for compliant quantitation workflows, Compound Discoverer software for advanced unknown identification and statistical analysis, the modular <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/483"><strong>TRACE 1600 Series GC</strong></a>, and the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/422"><strong>TriPlus RSH SMART robotic autosampler</strong></a>. Together, these components provide a highly automated, future-ready platform that maximizes uptime, simplifies maintenance through NeverVent and modular GC technologies, and delivers reliable HRAM data for both routine monitoring and advanced environmental research.</p></div></div></div></div></div></div></section></div></div></div></div></div></div></section>

News from LabRulezGCMS Library - Week 24, 2026

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Ioannes Marcus Marci Spectroscopic Society is a voluntary organization of scientific, scientific-pedagogical and professional workers in the field of spectroscopy, or legal entities engaged in scientific and application activities in this field, associated with joint activities. SSJMM was founded in 1949.

Spektroskopická společnost Jana Marka Marci

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Phenomenex is a global technology leader committed to developing novel analytical chemistry solutions that solve the separation and purification challenges of researchers in industrial, government and academic laboratories.

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News from LabRulezGCMS Library - Week 24, 2026

SPE Troubleshooting: Why Won't My Sample Flow Through the SPE Cartridge?

19th CSSC 2026: Early Bird Registration and Abstract Submission Deadline Approaching