Our Library never stops expanding. What are the most recent contributions to LabRulezICPMS Library in the week of 31th March 2025? Check out new documents from the field of spectroscopy/spectrometry and related techniques!<blockquote>👉 <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library">SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT SPECTROSCOPY/SPECTROMETRY 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://gcms.labrulez.com/library">LabRulezGCMS</a> libraries.</blockquote>This week we bring you application notes by Agilent Technologies and Shimadzu and other document by Thermo Fisher Scientific!<h3>1. Agilent Technologies: Enhanced RoHS Compliance Testing with Agilent <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library?manufacturerItems=1&amp;search=5800+ICP-OES&amp;sources=GCMS_EN-ICPMS_EN">5800 ICP-OES</a></h3>Accurate measurement of multiple elements including Cd, Cr, Pb, and Hg in plastic materials<ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_rohs_compliance_testing_5800_icp_oes_5994_8252en_agilent_d8b5f5a791.pdf">Full PDF for download</a></li></ul>The volume of waste electrical and electronic equipment (WEEE) is one of the fastest-growing waste streams worldwide. Over 62 million tonnes was generated globally in 2024.1 However, only a small fraction of this waste is properly recycled, contributing to environmental pollution and the loss of valuable materials. To address this issue and to improve the safety of electrical and electronic equipment (EEE), the EU first introduced the Restriction of Hazardous Substances (RoHS) directive in 2003.2 By restricting the use of specific hazardous materials such as lead, mercury, cadmium, hexavalent chromium, and certain flame retardants, RoHS helps ensure that products are safer for both consumers and the environment.3 As the design, type, and production of EEE evolve, ensuring compliance with RoHS regulations becomes increasingly challenging for manufacturers, importers, and distributors. Plastics, such as polyethylene (PE), polycarbonate, polystyrene, polyethylene terephthalate (PET), polyvinylchlorate (PVC), and acrylonitrile butadiene styrene (ABS), are often used in EEE because of their unique properties and cost-effectiveness.4 Manufacturers must rigorously test these materials using advanced analytical techniques to detect and quantify restricted substances, ensuring compliance with the stringent limits set by the directive. Among these techniques, Inductively Coupled Plasma Optical Emission Spectroscopy (ICP-OES) is one of the most effective tools for analyzing elements in plastics in accordance with RoHS regulations.5&nbsp;This application note describes a RoHS-compliant testing method for the multi-elemental analysis of plastics using an Agilent 5800 Vertical Dual View (VDV) ICP-OES. The methodology includes detailed procedures for sample preparation of a PE Certified Reference Material (CRM) and two real-life plastic materials used in EEE, instrument parameters, and performance evaluation. Quantitative results for arsenic (As), cadmium (Cd), chromium (Cr), lead (Pb), mercury (Hg), tin (Sn), antimony (Sb), sulfur (S), and zinc (Zn) are presented. The data set demonstrates the suitability of the method for supporting manufacturers in achieving RoHS compliance with a high level of efficiency and accuracy.<h4>Results and discussion</h4><h5>Sample analysis – spike recovery and precision&nbsp;</h5>Spike recovery tests in a sample matrix are an effective way to evaluate the reliability of the sample preparation and/or analytical methods, especially when suitable CRMs are unavailable. In this study, in addition to the analysis of the CRM, two real-life samples (A and B) were analyzed using the 5800 VDV ICP-OES. The measured concentrations of the analytes and spike recovery results are shown in Table 6. The spike recoveries for all analytes were within 94 to 108%, except for Sn in sample A, which had a spike recovery of 88%. This lower recovery could be due to the high measured concentration of Sn in sample A.&nbsp;However, the recovery of Sn in the CRM was 104%, assuring the method’s accuracy. The %RSD of the spike recovery measurements (n=3) was used to evaluate the method’s precision. As shown in Table 6, the spike recovery RSDs were ≤2.3% for all nine analytes in both samples A and B. This method validation data confirms the effectiveness of the microwave digestion sample preparation procedure for these materials. The results also demonstrate the excellent reproducibility and reliability of the 5800 VDV ICP-OES method for the analysis of complex plastic matrices.<h4>Conclusion&nbsp;</h4>The Agilent 5800 VDV ICP-OES was used for the quantitative analysis of nine elements including RoHS-specified elements, Cd, Cr, Pb, and Hg, in plastics that are typically used in electrical and electronic equipment (EEE). The samples included a plastic-based CRM (ERM-EC 681, polyethylene) and two real-life plastic matrices used in consumer electronics and electric vehicles. A one-stage microwave digestion sample preparation procedure ensured the complete digestion of these tough thermoplastic materials, facilitating accurate analysis by ICP-OES.&nbsp;The 5800 ICP-OES demonstrated outstanding sensitivity, accuracy, and stability, making it a reliable solution for EEE manufacturers required to comply with RoHS or equivalent testing standards. The Intelligent Rinse software feature of Agilent ICP Expert Pro streamlined operations by automatically adjusting rinse times based on user-defined thresholds, saving time and resources, and lowering the overall costs of analysis. This study highlights the 5800 ICP-OES instrument’s capability to deliver precise and consistent results, supporting the industry’s need for rigorous and reliable RoHS compliance testing.<h3>2. Shimadzu: Simultaneous Multi-Element Analysis of Farmland Soil ExtractsUsing the <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library?manufacturerItems=3&amp;search=ICPE-9820&amp;sources=ICPMS_EN">ICPE-9820</a>&nbsp;</h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_01_00815_en_bd40243933.pdf">Full PDF for download</a></li></ul><h4>User Benefits:</h4><ul><li>The ICPE-9820 can quickly analyze farmland soil for multiple elements simultaneously.</li><li>The ICPE-9820 can analyze high matrix samples without dilution, such as farmland soil solution extracts.</li></ul>Since soil contains constituents essential for crop growth that affect yield and quality, there is increasing demand for soil testing to help maintain optimum concentrations of soil constituents. Soil testing can determine the concentrations of these constituents and then create an optimized fertilization regimen to adjust them. Elemental analysis in soil testing is typically performed with an atomic absorption spectrophotometer (AAS). However, as soil testing becomes more common, there is a growing demand for faster soil analysis.&nbsp;The ICPE-9820, an inductively coupled plasma atomic emission spectrophotometer (ICP-AES) offers a wide dynamic range and can analyze multiple elements simultaneously. Soil testing analyzes soil for a large number of elements, and the ICPE-9820 can perform extremely efficient analyses that measure major and trace constituentssimultaneously.&nbsp;In this Application News, the ICPE-9820 analyzed farmland soil solution extracts for exchangeable constituents, available boron, trace elements and cadmium. And a spike recovery test and a dilution test were then performed to validate this analytical method.<h4>Conclusion&nbsp;</h4>In this Application News, the ICPE-9820 and extraction reagents normally used in soil testing were used to analyze three farmland soil solution extracts for exchangeable constituents, available boron, trace elements and cadmium. The results from validation testing show the analytical method was accurate. Using an axial view and radial view of plasma for different purposes allowed major constituents and trace constituents to be measured simultaneously without diluting samples for individual target analytes.<h3>3. Thermo Fisher Scientific: Driving productivity through reliable analysis with reduced complexity</h3><ul><li>Other document (case study)</li><li><a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/labrulez-bucket-strapi-h3hsga3/cs_003220_tea_icp_ms_icap_mx_series_element_cs003220_na_en_b888bf9432.pdf">Full PDF for download</a></li></ul>Element Material Testing Group is one of the world’s leading providers of testing, inspection, and certification. Element offers one of the most comprehensive ranges of materials testing services available in the Testing, Inspection, and Certification (TIC) sector that covers materials selection, application, and performance testing as well as failure analysis testing services. With over 9,000 employees and 270 laboratories, Element is providing their services worldwide to 55,000 customers working in diverse sectors including aerospace, energy, environmental, industrials, and life sciences.&nbsp;The Element Edmonton laboratory is ISO 17025 accredited, specializing in inorganic analysis. With three <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/products?category=228&amp;manufacturerItems=3">ICP-MS</a> and five<a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/products?category=251&amp;manufacturerItems=3"> ICP-OES</a> systems, it analyzes for inorganic metals in soils and waters. Typical clients come from different industries such as oil and gas, construction, agriculture, municipal drinking water, and many more.&nbsp;Alexsandra Robert is a senior scientist who has been working with the company for 20 years, with over 15 years of experience with ICP analysis. ICP-MS analyses performed at the Edmonton facility are primarily testing for heavy metal contaminant levels in soil and water. “As the primary production lab for Element in Alberta, we currently analyze over 40,000 soils and 15,000 waters annually for metals,” stated Alexsandra.&nbsp;Analysis of soils and waters for elemental contaminants or minerals is typically performed using either Inductively Coupled Plasma – Optical Emission Spectroscopy (ICP-OES) or Inductively Coupled Plasma – Optical Mass Spectroscopy (ICP-MS) to satisfy the different analytical and regulatory requirements of customers. “The choice between ICP-OES and ICP-MS is largely driven by factors such as required detection limits, number of analytes, regulatory guidelines, and type of information requested by our clients,” Alexsandra further illustrated.Busy analytical testing laboratories experience tremendous workloads and need to ensure that reliable results are delivered to their valued customers in time. Alexsandra noted, “Achieving reliable analytical results with minimum time and resources is very critical to the overall success of any analytical laboratory.” A Thermo Scientific™ <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/products/1487">iCAP™ MSX ICP-MS</a> driven by Thermo Scientific™ <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/products/1489">Qtegra™ Intelligent Scientific Data Solution Software</a> was added to the instrumental portfolio of the Element laboratory in Edmonton and has been in use for testing of environmental samples including ground waters, lake waters, surface waters, and different types of soil samples. Whereas the analysis of water samples is relatively straightforward, soil samples need to be acid digested either by microwave or hot plate digestion before introducing them into the ICP-MS for analysis. Samples are typically diluted off-line prior to analysis using ultrapure diluent to ensure that total dissolved solids in samples do not exceed the tolerance level of ICP-MS instruments. Alexsandra provided insight on the typical workflow of an environmental laboratory, “For laboratories analyzing hundreds of samples every day, off-line liquid dilution is a tedious, error-prone, and expensive analytical step as it requires time, manual intervention, and expensive reagents and apparatus.”

News from LabRulezICPMS Library - Week 14, 2025

News from LabRulezICPMS Library - Week 16, 2025

As countries across the world accelerate their efforts to move away from fossil fuels, lithium-ion batteries have rapidly become established as a key component in the drive to greener energy alternatives. But lithium is only part of the story. In this blog post, I’ll review the role that lithium and other elements play in battery technology, discuss how these elements can be quantified and assess what potential options there are for future developments in this area.<h3>Lithium ion batteries – their promise and their problems</h3>Lithium ion battery cathodes are typically made from a mixed metal oxide base to which lithium is added and, usually, nickel, cobalt and manganese oxides are used for this purpose. To maintain optimum performance and to slow degradation of cathode materials over multiple charging and discharging cycles as much as possible, these materials need to be highly purified. In particular, they must be free of metal impurities (particularly iron and vanadium) and sulphur, as these elements disrupt battery performance and accelerate degradation processes. Lithium ion batteries have become a central focus for power generation for electric vehicles and portable devices because they offer high-power storage capacity for their size and good charge/discharge cycling stability over a relatively long time period. However, there are safety concerns surrounding lithium ion batteries, as they can spontaneously ignite and subsequently explode as a result of overheating.This overheating can be caused by factors such as electrical shorting, rapid discharge, overcharging or mechanical damage, so considerable research and development in recent years has been focused on making them as safe as possible. Safety is not the only problem for batteries based on lithium. Although the price of lithium batteries has decreased significantly (by almost 90% between 2010 and 2020, according to some estimates1), since January this year, the price of lithium raw materials (primarily lithium carbonate and lithium hydroxide) has been rising steadily. Lithium is not a limitless resource on Earth — it’s present at levels of only between 0.002 – 0.006 wt% in the Earth’s crust — so as demand ramps up, supply will diminish and costs will rise. The cost is not only a financial one. Mining activities will need to sharply increase if dependence on lithium is maintained, which will significantly impact the environment in areas where lithium deposits are rich enough for mining to be viable. This, however, also means that recycling and reprocessing of spent batteries will become an essential part of the lithium battery cycle.<h3>Are there alternative metal ion technologies to lithium?</h3>In the initial stages of lithium ion battery research in the 1970s and early 1980s, the potential of sodium ion batteries was also investigated.2 Sodium has the considerable benefit of being much more widely available than lithium — it’s the seventh most abundant element, with an average concentration of 2.27% by weight in the Earth’s crust — and so cheaper and more viable to extract from almost anywhere. However, it soon became clear at the time that the power density and charge/discharge cycling stability of sodium ion batteries was not as good, in part because the larger ionic radius of sodium means that the graphite anodes that are efficiently used with lithium ion batteries cannot be used with sodium batteries. As a result, sodium battery research languished for many years until, in the early 2010s, interest in this area resurged because of increasing battery demand and the discovery that hard carbon3 provided better anode performance with sodium ions. There is still a long way to go with sodium ion battery development, but promising advances are happening now. In June 2020, researchers from Washington State University (WSU) and the Pacific Northwest National Laboratory (PNNL) announced that they had developed a viable sodium ion battery4, and Stanford University is spearheading research into new sodium ion-based battery materials.5<h3>Measuring lithium and other metals involved in battery technology</h3>It’s clear that accurate determination and quantification of both the cathode metal oxide elements and trace impurities in the cathode material are of key importance for advancing and scaling up battery production, research and development. The techniques that are available for this analysis include <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/products?category=251&amp;manufacturerItems=3">inductively coupled plasma optical emission spectrometry (ICP-OES)</a> and <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/products?category=232&amp;manufacturerItems=3">inductively coupled plasma mass spectrometry (ICP-MS)</a>, and recently, the applications team at Thermo Fisher Scientific’s Bremen, Germany, facility have produced an application note on <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_73872_icp_oes_elements_lithium_batteries_an73872_en_691a4c3f8a.pdf">analysis of trace elements in lithium batteries</a> using the <a target="_blank" rel="noopener noreferrer" href="https://www.thermofisher.com/order/catalog/product/BRE0020758#/BRE0020758">Thermo Scientific™ iCAP™ PRO XP ICP-OES</a>. If you’d like to learn more about how these and other technologies that can support battery technology advancements, take a look at our batteries resources page <a target="_blank" rel="noopener noreferrer" href="https://www.thermofisher.com/batteries">here</a>.

Is Battery Technology Just All About Lithium?

Our Library never stops expanding. What are the most recent contributions to LabRulezICPMS Library in the week of 19th May 2025? Check out new documents from the field of spectroscopy/spectrometry and related techniques!<blockquote>👉 <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library">SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT SPECTROSCOPY/SPECTROMETRY 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://gcms.labrulez.com/library">LabRulezGCMS</a> libraries.</blockquote>This week we bring you other document by Agilent Technologies, guide by Shimadzu and brochure by Thermo Fisher Scientific!<h3>1. Agilent Technologies: 5 Reasons You Need Onsite Metals Analysis Capabilities for Battery Recycling</h3><ul><li>Other document</li><li><a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/labrulez-bucket-strapi-h3hsga3/quickref_battery_recycling_infographic_icp_oes_5994_8002en_agilent_024ec4b399.pdf">Full PDF for download</a></li></ul>1. Monitoring airborne particulates&nbsp;Mechanical separation e.g. shredding, creates airborne particulates, hazardous to human health and the environment. ICP-OES can be used to monitor air filters to ensure regulatory compliance.&nbsp;2. Analyzing black mass&nbsp;The powder from separation, known as “black mass”, is widely refined through hydrometallurgical and pyrometallurgical processes. ICP-OES effectively measures impurities to ensure the final product quality meets specifications.&nbsp;3. Monitoring and optimizing recycling processes&nbsp;Efficient separation is vital for effective downstream processing. Onsite ICP-OES enables real-time monitoring and optimization at each stage, maximizing material recovery like feedstock chemicals.&nbsp;4. Ensuring QC of input chemicals&nbsp;Purity of chemicals used in battery recycling is crucial to avoid introducing contaminants in the final product. For example, leaching – a common purification step – uses strong acids and solvents to isolate compounds.5. Monitoring environmental discharges&nbsp;Thorough chemical analysis of emissions and waste can be achieved using ICP-OES to ensure the correct and safe disposal of these by-products.<h3>2. Shimadzu: Application Data Book - Polymer and Electronic Material</h3><ul><li>Guide</li><li><a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/labrulez-bucket-strapi-h3hsga3/c160_e010_c8512bcb71.pdf">Full PDF for download</a></li></ul>The Shimadzu "Thermal Analysis 60 Series Application Data Book" is a comprehensive technical compendium showcasing the use of Shimadzu thermal analysis instruments—primarily the<a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library?manufacturerItems=3&amp;search=+DSC-60"> DSC-60</a>, <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library?manufacturerItems=3&amp;search=DTG-60">DTG-60</a>, and <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library?manufacturerItems=3&amp;search=TGA-50">TGA-50</a>—for analyzing a wide array of polymeric and electronic materials. This application-focused book is structured into several sections that highlight practical case studies across categories such as plastics, electronic materials, and battery components, demonstrating how thermal techniques can be used to measure melting behavior, crystallization, decomposition, and glass transition properties.In the section dedicated to plastics, studies examine the thermal responses of materials such as PET, PEEK, nylon, polypropylene, and polyimide. The influence of thermal history on crystallinity and thermal stability is highlighted through differential scanning calorimetry (DSC) analyses. For instance, the book explains how rapid cooling affects PET’s amorphous structure and how glass transition shifts depending on sample morphology and processing history. Shimadzu’s DSC-60 is used throughout to detect transitions such as glass transitions and melting points with high sensitivity and resolution.When analyzing electronic materials, the book includes examples such as thermal decomposition of diodes and quantification of quartz in epoxy resins. Using Shimadzu’s DTG-60, these analyses reveal how semiconductor components decompose and how fillers like quartz contribute to thermal resistance. Similarly, for lead-free solder materials, melting behavior is compared to traditional Sn-Pb alloys, emphasizing the importance of composition in defining thermal performance—a critical aspect in electronics manufacturing.The section on battery and fuel cell materials underscores the role of thermal analysis in energy-related applications. Using the DSC-60, separators in lithium-ion batteries are examined for their melting characteristics, which are crucial for safety mechanisms. The book also delves into analyzing Nafion® membranes for polymer fuel cells, using DSC to interpret water cluster dynamics that influence conductivity. These examples collectively illustrate how Shimadzu’s thermal analysis instruments provide valuable insights into the thermal behavior of modern materials used across diverse industries.<h3>3. Thermo Fisher Scientific: Thermo Scientific <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/products/1715">iSC-65 Autosampler</a> and <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/products/1489">Qtegra ISDS Software</a>: reliability to power through your challenging ICP-OES and ICP-MS workflows</h3><ul><li>Brochure</li><li><a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/labrulez-bucket-strapi-h3hsga3/sl_001587_tea_isc_65_autosampler_and_qtegra_isds_software_sl001587_en_0809719473.pdf">Full PDF for download</a></li></ul>The <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/products/1715">Thermo Scientific™ iSC-65 Autosampler</a>, controlled by <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/products/1489">Thermo Scientific™ Qtegra™ Intelligent Scientific Data Solution™ (ISDS) Software</a>, is a robust, feature-rich sample introduction system with advanced hardware and software capabilities designed to improve productivity and profitability in your routine workflow.&nbsp;The iSC-65 Autosampler is compatible with the Thermo Scientific™ <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/products?category=231&amp;manufacturerItems=3&amp;search=icap+pro+icp-oes">iCAP™ PRO Series ICP-OES</a> and iCAP™ Qnova Series ICP-MS instruments. It is ideally suited for use in applications in environmental, food, industrial, battery technology, sustainable fuels, petrochemical, and pharma markets that require reliable sampling over extended periods.&nbsp;<h5>Key hardware features&nbsp;</h5><ul><li>An industry-proven three-axis screw thread design reliably drives the sample probe with sub mm accuracy and precision.&nbsp;</li><li>Materials that are resistant to common chemicals and acid are used throughout, allowing for reliable, contamination-free operation over extended periods.&nbsp;</li><li>Up to four industry standard sample racks can be installed at one time. Racks with vial capacities of 21, 24, 40, 60, and 90 are supported.&nbsp;</li><li>A dedicated area for 50 mL (either flat or round base) tubes is provided, ideal for solutions that need to be repeatedly analyzed, for example, quality control standards.</li><li>In case of accidental spillage, the sample rack tray can be removed, and fittings are provided to support either a gravity drain to the front or a pumped drain to the rear of the iSC-65 Autosampler.&nbsp;</li><li>The two-channel rinse station is fed by a dedicated rinse pump that can be used to remove excess rinse solution or fitted to a gravity drain. The rinse station is removable for cleaning and is connected to tubing with luer style fittings for ease of use and peace of mind.&nbsp;</li></ul><h5>Key sampling capabilities&nbsp;</h5><ul><li>Step Ahead – sends the probe to the rinse station during data acquisition, using the sample volume in the probe and transfer tubing to complete the analysis. Less sample solution is required, decreasing waste and instrument wear, and less time is required to rinse, reducing rinse solution usage and accelerating sample throughput. &nbsp;</li><li>Flexible sampling depths – vial-specific probe depths enable correct sampling to avoid suspended particles that could otherwise lead to blockages, minimizing maintenance and potential exchange of sample introduction components.</li></ul><h5>Software features built on hardware capabilities&nbsp;</h5><ul><li>The Thermo Scientific iSC-65 Autosampler is controlled through a dedicated software plug-in within the Qtegra ISDS Software platform. A high clarity, easy to follow, visual workflow is carried through multiple views.&nbsp;</li><li>A dedicated view for the iSC-65 Autosampler is accessible in the Qtegra ISDS Software Dashboard that provides access to common autosampler actions – probe movement, pump speed control, etc.</li></ul>

News from LabRulezICPMS Library - Week 21, 2025

This study presents a combined microwave-assisted digestion (MAD) and dispersive magnetic solid-phase microextraction (DMSPE) method for determining major (Ca, Cu, Fe, Mn, Mg, Na, Zn) and trace elements (As, Pb, Se) in lignocellulosic biomass by ICP-OES. Maghemite nanoparticles were synthesized and characterized to serve as sorbents, and conditions for both MAD and DMSPE were optimized using a central composite design.The method achieved low detection limits (As 0.01, Pb 0.03, Se 0.01 µg g–1) and high enrichment factors (21–42 for trace elements). Validation with certified reference materials confirmed accuracy. Application to five biomass samples provided reliable quantification of major elements, while As, Pb, and Se were below LOQs. This approach offers a robust strategy for elemental profiling of lignocellulosic biomass.<blockquote><h4>The original article</h4><h4><a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/10.1021/acsomega.5c02196">Microwave-Assisted Digestion Method and Dispersive Magnetic Solid-Phase Microextraction for the Determination of Major and Trace Elements in Lignocellulosic Biomass by ICP-OES</a></h4>Camilla M. Belmiro, Mikaelle de Carvalho Gomes, Fernanda Nunes Ferreira, Márcia Angelica F. S. Neves, and Jefferson Santos de Gois*ACS Omega 2025, 10, 28, 30443–30449<a target="_blank" rel="noopener noreferrer" href="https://doi.org/10.1021/acsomega.5c02196">https://doi.org/10.1021/acsomega.5c02196</a><h6>licensed under <a target="_blank" rel="noopener noreferrer" href="https://creativecommons.org/licenses/by/4.0/">CC-BY 4.0</a></h6></blockquote>Selected sections from the article follow. Formats and hyperlinks were adapted from the original.Lignocellulosic biomass consists mainly of cellulose, hemicellulose, and lignin. It can be used as an ecological material for the production of second-generation fuels, such as ethanol from petroleum to replace fossil fuels and their derivatives, and as an energy source (by gasification, pyrolysis, liquefaction, or combustion), with the aim of contributing to the reduction of global CO2 emissions. <a href="javascript:void(0);">(1−4)</a>A variety of analytical techniques can be used for the elemental characterization of biomass and biomass-derived ash, such as inductively coupled plasma mass spectrometry (ICP–MS), <a href="javascript:void(0);">(5,6)</a> flame atomic absorption spectrometry (FAAS), <a href="javascript:void(0);">(7)</a> graphite furnace atomic absorption spectrometry (GF AAS), <a href="javascript:void(0);">(3)</a> laser-induced breakdown spectroscopy (LIBS), <a href="javascript:void(0);">(8)</a> and inductively coupled plasma optical emission spectrometry (ICP-OES). <a href="javascript:void(0);">(9−11)</a>Inductively coupled plasma optical emission is often used for the determination of trace elements due to its low detection limits and multielement capability. However, this technique usually requires at least one sample preparation step to solubilize the analytes in an aqueous medium prior to analysis. Microwave-assisted acid digestion (MAD) in closed vessels is considered the most efficient technique for the decomposition/solubilization of organic sample matrices and the determination of trace elements by spectrometric techniques. <a href="javascript:void(0);">(12)</a> Concentrated acids and their mixtures have been identified for the preparation of biomass samples with MAD, the most commonly used acids are hydrofluoric acid, <a href="javascript:void(0);">(10)</a> nitric acid, and/or hypochlorous acid and their mixtures; <a href="javascript:void(0);">(13)</a> hydrogen peroxide may also be used to recycle oxygen into the aqueous media. <a href="javascript:void(0);">(4,6)</a>Elements such as As, Pb, and Se usually occur in very low concentrations (ng g–1) and therefore require very sensitive analytical techniques for their determination or preconcentration methods, which can provide a cost-effective method for their determination. Dispersive magnetic solid-phase extraction (DMSPE) with magnetic nanoparticles of iron oxide (Fe3O4 and Fe2O3) is advantageous because they can be quickly obtained by synthesis, can adsorb elements, and can be easily separated from the aqueous medium with a magnet. <a href="javascript:void(0);">(14,15)</a>Therefore, the aim of this work was to develop a MAD method using diluted HNO3 for the determination of trace elements (Ca, Cu, Fe, Mn, Mg, Na, Zn), followed by an MSPE preconcentration method for the determination of As, Pb, and Se in lignocellulosic biomass samples by ICP-OES.<h4>2. Materials and Methods</h4><h5>2.1. Instrumentation</h5>An ICP-OES model iCAP 6300, equipped with a Mira Mist nebulizer (Burgener Research Inc., Canada) and a cyclone spray chamber (Thermo Scientific, USA), was used for the multielement determination. The operating parameters used in ICP-OES were plasma gas flow (12 L min–1), nebulizer gas flow (0.4 L min–1), auxiliary gas flow (1.0 L min–1), radio frequency power (1300 W), pump flow rate (5 rpm, 0.2 mL min–1), and radial view. The monitored wavelengths were Ca (422.673 nm), Cu (324.754 nm), Fe (259.940 nm), Mn (257.610 nm), Mg (280.270 nm), Na (588.995 nm), Zn (213.856 nm), As (189.042 nm), Pb (220.353 nm), Se (203.985 nm), and Sc (361.384 nm) as internal standards. Argon with a purity of 99.95% (Air Liquide, Brazil) was used as the main, auxiliary, and nebulizer gas. All mass measurements were performed using an analytical balance with an accuracy of 0.1 mg, model M214A (Bel Engineering, Italy). The samples were ground in a mill model MG200 (Black+Decker, Brazil) and sieved with a 200 mesh sieve.The microwave-assisted digestion of the samples was carried out in a <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library?mainauthorItems=444&amp;search=Multiwave+PRO">Multiwave PRO microwave oven</a> (Anton-Paar, Graz) with a 24HVT50 rotor model. The DMSPE experiments were carried out in a horizontal orbital shaker model SK-180-PRO (Scilogex, EUA) and a thermal shaker model Thermo Mixer (Kasvi, Brazil).<h5>2.5. Dispersive Magnetic Solid-Phase Microextraction Procedure</h5><h5>2.5.2. Characterization of the γ-Fe2O3 Magnetic Nanoparticles</h5>The synthesized magnetic γ-Fe2O3 nanoparticles were characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), field emission scanning electron microscopy (FEG-SEM), and thermogravimetric analysis (TGA). A Frontier FTIR of the 98737 series (PerkinElmer, USA) was used for the FTIR analysis. The analysis was performed with a resolution of 4 cm–1 in the range of 4000 to 400 cm–1 in KBr pellets. For TGA, an SDT Q600 model (TA Instruments, USA) was used with the following parameters: a temperature range from 30 to 700 °C at a rate of 20 °C min–1 under a nitrogen atmosphere (150 mL min–1). For FEG-SEM, images were taken with an electronic microscope model JSM-7100F (Jeol, Japan) with magnifications of x30 000 and x60,000. The XRD was carried out in an AXS D-5005/Siemens (Bruker, EUA), with an angular step of 0.10°, ranging from 15 to 70°, and with an acquisition time between counts of 1.0 s.<h4>3. Results and Discussion</h4><h5>3.1. Chemical Characterization of the γ-Fe2O3 Magnetic Nanoparticles</h5>The X-ray diffractogram of the magnetic γ-Fe2O3 nanoparticles is shown in <a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/10.1021/acsomega.5c02196#fig1">Figure 1</a>A. Diffraction peaks were consistent with the standard structure and indicated the presence of the cubic phase of maghemite. These reflections are assigned to (220), (311), (400), (422), (511), and (440), which correspond to the crystallographic planes that are characteristic reflections of maghemite, indicating that they are consistent with the X-ray diffraction pattern of γ-Fe2O3. <a href="javascript:void(0);">(17)</a><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/ACS_Omega_2025_10_28_30443_30449_Figure_1_X_ray_diffraction_A_Fourier_transform_infrared_spectra_B_scanning_electron_microscopy_x60_000_C_and_thermogravimetric_analysis_of_g_Fe2_O3_D_8bb288c909.jpg" alt="ACS Omega 2025, 10, 28, 30443–30449: Figure 1. X-ray diffraction (A), Fourier transform infrared spectra (B), scanning electron microscopy x60,000 (C), and thermogravimetric analysis of γ-Fe2O3 (D)." srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_ACS_Omega_2025_10_28_30443_30449_Figure_1_X_ray_diffraction_A_Fourier_transform_infrared_spectra_B_scanning_electron_microscopy_x60_000_C_and_thermogravimetric_analysis_of_g_Fe2_O3_D_8bb288c909.jpg 238w," sizes="100vw" width="1750" height="1144">Fourier transform infrared spectroscopy was used to characterize the functional groups. The FTIR spectra of the γ-Fe2O3 nanoparticles, shown in <a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/10.1021/acsomega.5c02196#fig1">Figure 1</a>B, highlight the bands at 628, 580, and 447 cm–1, which correspond to the vibrational mode of stretching and angular deformation characteristic of Fe–O bonding and confirm the formation of γ-Fe2O3. <a href="javascript:void(0);">(18)</a> The broad stretching band at 3411 cm–1 corresponds to the OH group and surface H2O, and the band at 1630 cm–1 correlates with the angular deformation mode of H–O–H. The OH groups at the surface are associated with residual or physically adsorbed water. <a href="javascript:void(0);">(14)</a>The thermal stability of maghemite was investigated using TGA. It was found that the material is thermally stable, as it suffers a slight mass loss with an increase in temperature, as shown in <a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/10.1021/acsomega.5c02196#fig1">Figure 1</a>D. The mass loss at around 100 °C is due to the loss of water, which is physically adsorbed onto the material. <a href="javascript:void(0);">(16)</a> In the range between 550 and 580 °C, a mass loss is observed, which is due to phase transitions from maghemite to hematite. <a href="javascript:void(0);">(15)</a><h5>3.2. Microwave-Assisted Digestion of Biomass</h5>Microwave-assisted digestion is a powerful technique for decomposition of the organic matrix of a sample and solubilization of inorganic analytes into the aqueous media for analysis. This technique can be used with inorganic acids and H2O2 to increase the efficiency of sample digestion. Microwave-assisted digestion in closed vessels can minimize analyte loss, reduce contamination, and shorten sample preparation time. It also offers high sample decomposition efficiency and high sample throughput. <a href="javascript:void(0);">(19,20)</a> The selection of the type and concentration of inorganic acids, as well as the sample mass, is crucial for sample preparation in microwave-assisted digestion. Therefore, the optimization of these factors was performed, as described in Section <a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/10.1021/acsomega.5c02196#sec2_3">2.3</a>. Nitric acid was selected for sample preparation due to its oxidizing properties and versatility for a variety of organic matrices; furthermore, the nitrates are soluble in aqueous media.<a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/suppl/10.1021/acsomega.5c02196/suppl_file/ao5c02196_si_001.pdf">Table S3</a> shows the fitted models for each analyte after refinement, where the obtained R-squared ranged from 0.6885 to 0.9989, while the fitted R-squared ranged from 0.6719 to 0.9987, indicating a good fit of the models. According to the Shapiro–Wilk test (α = 0.05), the residuals of the models for Ca, Fe, Mg, Mn, Na, and Zn were found to follow a normal distribution, except for Cu, for which the central limit theorem was considered.The desirability function was applied to determine the optimal experimental condition for multiresponse optimization, with values ranging from 0 (undesirable value) to 1 (desirable value). <a href="javascript:void(0);">(21)</a> The surface response of the overall desirability for the microwave-assisted digestion method is shown in <a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/10.1021/acsomega.5c02196#fig2">Figure 2</a>. The optimum experimental condition was achieved at a sample mass of 280 mg, 2.5 mL of HNO3, and 2.0 mL of H2O2, achieving an overall desirability of 0.534, which is an acceptable value, while the individual desirabilities were Ca (0.618), Cu (0.535), Fe (0.428), K (0.388), Mg (0.378), Mn (0.866), Na (0.620), and Zn (0.591).<img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/ACS_Omega_2025_10_28_30443_30449_Figure_2_Overall_desirability_response_surface_for_the_optimization_of_the_microwave_assisted_digestion_of_lignocellulosic_biomass_9dd074f965.jpg" alt="ACS Omega 2025, 10, 28, 30443–30449: Figure 2. Overall desirability response surface for the optimization of the microwave-assisted digestion of lignocellulosic biomass and determination of Ca, Cu, Fe, Mn, Mg, Na, and Zn by ICP-OES." srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_ACS_Omega_2025_10_28_30443_30449_Figure_2_Overall_desirability_response_surface_for_the_optimization_of_the_microwave_assisted_digestion_of_lignocellulosic_biomass_9dd074f965.jpg 245w," sizes="100vw" width="1305" height="420"><h4>4. Conclusions</h4>A microwave-assisted digestion method and a dispersive magnetic solid-phase microextraction method for trace-element determination in lignocellulosic biomass were successfully obtained. Both methods were optimized using a multivariate approach, which ensured a high efficiency of the methods.The developed microwave-assisted digestion achieved good accuracy using a lower concentration of reagents than reported in the literature, while the microextraction method using maghemite nanoparticles provided a simple and reliable alternative for the determination of trace elements in biomass samples. Although only Ca, Cu, Fe, Mn, Mg, Na, Zn, As, Pb, and Se were considered in the validation of the method, we believe that this method can be extended for other analytes after proper validation, especially As, Pb, and Se, since the recovery of the analytes was performed by dissolving the nanomaterial into an aqueous medium. The methods provided good accuracy for all analytes and LOQs suitable for the purpose and proved to be a good alternative for the determination of trace elements in biomass samples from lignocellulose.

Microwave-Assisted Digestion Method and Dispersive Magnetic Solid-Phase Microextraction for the Determination of Major and Trace Elements in Lignocellulosic Biomass by ICP-OES

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