News from LabRulezICPMS Library - Week 45, 2026

Our Library never stops expanding. What are the most recent contributions to LabRulezICPMS Library in the week of 2nd November 2026? Check out new documents from the field of spectroscopy/spectrometry and related techniques!

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1. Agilent Technologies: ICP-MS Elemental Impurity Analysis of Pharmaceuticals Following USP and ICH Protocols

Routine oral drug analysis using the Agilent 9500 Triple Quadrupole ICP-MS in Advanced Helium Mode

• Application note
• Full PDF for download 

All pharmaceutical products must be evaluated to demonstrate that they are safe for patients and effective for their intended therapeutic use. As part of this evaluation, potentially toxic elemental impurities must be monitored. The relevant requirements and procedures are specified by organizations such as the United States Pharmacopeia (USP) and the International Council for Harmonisation of Technical Requirements (ICH). ICH Q3D(R2) establishes Permitted Daily Exposure (PDE) values for 24 elements and includes the elements specified in USP General Chapter <232>.^1,2 USP General Chapter <233> describes the analytical procedures and validation requirements for determining elemental impurities.³ In this study, the 24 elements listed in ICH Q3D(R2) were analyzed using an ICP-MS method based on USP <233> to meet the requirements of both ICH and USP.

Agilent ICP-MS systems, including single quadrupole (SQ) and triple quadrupole (QQQ) instruments, have been extensively tested and used in pharmaceutical laboratories for many years.4 The instruments deliver reliable, high-quality data, supported by trusted service teams, qualification services, and compliance solutions. To extend the benefits of ICP‑QQQ technology to a wider range of laboratories, Agilent has developed the 9500 ICP-QQQ, an entry-level triple quadrupole ICP-MS.⁵ Unlike traditional ICP-QQQ systems, which are often used for advanced applications, the 9500 is designed for routine sample analysis. It combines excellent interference removal, dependable performance, and straightforward operation, enabling laboratories to benefit from ICP‑MS/MS capability in high‑volume daily workflows while still supporting more complex research projects. 

Agilent 9500 Triple Quadrupole ICP-MS 

The 9500 ICP-QQQ is equipped with the Dual-Cell System (DCS), a new collision/reaction cell (CRC) that incorporates two independently controlled ion guides. The DCS enables effective removal of many spectral interferences through a new standard cell-gas mode, Advanced Helium Mode (AHM), which uses Kinetic Energy Discrimination (KED) and Collision-Induced Dissociation (CID) mechanisms.⁶ This enhanced helium (He) mode provides efficient removal of polyatomic interferences while maintaining sufficient high sensitivity in the low-mass range, making it suitable for the analysis of most analytes in the majority of sample types. 

AHM replaces the need for conventional multitune operation using no gas, He, and high energy (HE)He modes. By eliminating gas switching between these modes, AHM simplifies operation and improves sample throughput. 

In pharmaceutical samples, AHM is particularly advantageous for the analysis of elements such as lithium (Li), which typically has low sensitivity in conventional He mode, as well as vanadium (V), chromium (Cr), arsenic (As), and selenium (Se), which are susceptible to polyatomic interferences. 

While AHM effectively resolves many polyatomic ion interferences, such as oxide ions (MO+ ) and argon-based ions (ArM+ ), it is less effective at suppressing doubly charged ion interferences (M++). However, a reactive cell gas mode known as Air cell mode has been developed for the 9500 that reduces M++ interferences through ion–molecule reactions with oxygen (O2 ).7 In Air cell mode, ambient air is purified through an air filter before being introduced into the cell. Using MS/MS settings to control which analyte ions enter the DCS and interact with O2, the 9500 ICP-QQQ ensures effective interference removal of M++, as well as challenging polyatomic species that AHM cannot fully suppress.

This note describes the analysis of 24 elements in an over-the-counter (OTC) oral drug product using the 9500 ICP-QQQ in AHM. The method was evaluated for both limit and quantitative procedures against the performance criteria specified in the ICH guidance and USP Chapters.

Conclusion 

A rapid method for the simultaneous determination of the 24 elemental impurities specified in ICH Q3D (R2) was successfully developed using the Agilent 9500 Triple Quadrupole ICP-MS. Operating the 9500’s Dual-Cell System (DCS) in Advanced Helium Mode (AHM) effectively suppressed polyatomic interferences while maintaining sufficient sensitivity across the entire mass range. This performance enabled quantification of all target elements in an oral drug product using a single gas mode. Eliminating conventional multitune operation and gas switching also enabled a faster and more streamlined ICP‑MS workflow. 

The method was evaluated in accordance with the requirements of USP <233>, including detectability, precision, intermediate precision, specificity, and accuracy. All 24 elements met the applicable acceptance criteria. The RSDs for the primary isotopes were less than 3% in the precision study, and results obtained on different days met the intermediate precision criterion. Acceptable recoveries were obtained at all evaluated spike levels from 0.3 to 1.5 J. 

AHM provided low detection limits and background equivalent concentrations for all 24 elements, including V, Cr, As, and Se, which are susceptible to polyatomic interferences arising from the sample matrix. These results demonstrate effective interference removal capability and quantitative performance of the method. The use of a preset USP/ICH method in the Agilent OpenLab ICP-MS software further simplified method setup and routine operation. 

In addition, Air cell mode provides a complementary massshift approach for specific sample matrices affected by spectral interferences that cannot be sufficiently resolved using AHM alone. Examples include doubly charged rare earth element ion interferences on As and Se. 

Overall, the 9500 ICP-QQQ method using AHM met the requirements of both ICH and USP for the determination of elemental impurities in the OTC drug sample. The ability to accurately determine the target elements at 0.3 J confirms that the method is suitable for monitoring elemental impurities at concentrations as low as 30% of the J value. 

The single-mode analytical approach simplifies operation, reduces analysis time, and improves sample throughput, making it suitable for routine pharmaceutical analysis.

2. LECO: Metallography of Lithium-Ion Battery Coated Foils

• Application note
• Full PDF for download

As the demand for renewable energy and green technologies accelerates, companies are prioritizing powerful, efficient, and reliable energy storage solutions. Lithium-ion batteries have rapidly become the leading clean energy choice across automotive, defense, and stationary storage applications. Most lithium-ion cells use a graphite anode paired with either a Lithium Iron Phosphate (LFP) or Lithium Nickel Manganese Cobalt (NMC) cathode. During manufacturing, the anode and cathode slurries are coated onto thin metal foils, which makes metallographic inspection a critical quality control step. Metallography enables precise evaluation of key battery performance factors, including adhesion, coating and foil thickness, and porosity. These characteristics directly influence charge-discharge efficiency, energy density, and overall safety, helping manufacturers prevent defects that could otherwise lead to performance loss or hazardous failures.

Understanding Battery Foil Coating 

Thickness measurements of anode and cathode coatings are essential for preventing downstream issues such as reduced battery efficiency, shortened battery life, and the risk of thermal runaway. Irregular coatings can generate localized hotspots that worsen with every charge– discharge cycle. To minimize manufacturing waste and maintain quality, it is recommended to check coating thickness at multiple stages of the production process. 

These measurements reveal uniformity and flatness across the foil. The material should be evenly distributed with homogeneous particle dispersion and be free of defects such as holes, cracks, delamination, or scratches. By monitoring thickness in real time, manufacturers can adjust parameters, such as coating speed or calendering gaps, to optimize performance and improve overall process efficiency.

Image Analysis for Coating Thickness Measurements 

LECO's image analysis software, PAX-it, provides users with an enhanced user interface to automate and generate reports based on common metallographic inspections for coated foils, including coating and layer thicknesses. Samples in the as-polished condition are suitable for observation and these measurements (Figure 7). 

With the “Measurement Sequence” capability, users can repeatedly measure thicknesses from a captured image (Figure 8). The Measurement Sequence is set up to prompt an operator to make measurements based on predefined parameters and locations. It is often recommended to use multiple measurements and areas of a sample for an accurate average of the entire layer of interest (Figure 9). Pass/Fail criteria can be established to alert a user if any of the measurements don't meet quality standards. This can also be used to observe any coating inconsistencies, like porosity or inclusions, that could lead to failure. Users also have the option to customize and print out Excel reports for traceability purposes.

Conclusion 

Metallographic inspection is a critical quality control tool in lithium-ion battery manufacturing, directly impacting performance, safety, and reliability. Accurate evaluation of coating thickness, adhesion, and uniformity on anode and cathode foils helps prevent efficiency losses, premature failure, and safety risks such as thermal runaway. Because these foils are highly sensitive to deformation, careful sectioning, delicate cold mounting, and controlled grinding and polishing are essential to preserve the true microstructure. LECO's recommended preparation methods and consumables enable consistent, deformation-free surfaces suitable for precise analysis. When combined with PAX-it image analysis software, manufacturers can reliably measure coating and foil thickness, detect defects, and generate traceable reports. Overall, a well-controlled metallographic workflow supports optimized process control, reduced manufacturing waste, and the production of safer, higherperforming lithium-ion batteries.

3. Metrohm: Automated quality control of diesel using near-infrared spectroscopy

• Application note
• Full PDF for download

Key parameters for diesel fuel quality testing include the cetane index (ASTM D613), flash point (ASTM D56), density (ASTM D975), T95 (ISO 3405), and viscosity at 40 °C (ISO 3104). Usually, determining these properties is labor intensive and time consuming, requiring multiple analytical techniques and dedicated instrumentation. The OMNIS NIR Analyzer Liquid provides a fast, reliable, and reagentfree solution to simultaneously determine these diesel fuel properties without sample preparation. The precise temperature control ensures that all samples are measured in compliance with ASTM D8340, ASTM D8321, and ASTM D6122. Combined with the OMNIS Sample Robot M – NIR, the system offers fully automated operation for maximum lab efficiency.

EXPERIMENTAL EQUIPMENT 

Diesel samples were measured with an OMNIS NIR Analyzer Liquid (Figure 1) in transmission mode over a wavelength range of 1000–2250 nm. Reproducible spectrum acquisition was achieved using the built-in temperature control at 30 °C. An OMNIS Sample Robot M – NIR was used for fully automated sample measurement with disposable vials (8 mm pathlength). The vials are closed, which reduces the flammability risk for fuel samples to an absolute minimum. OMNIS Software was used for all data acquisition and prediction model development.

CONCLUSION

This Application Note shows the feasibility of using NIR spectroscopy for the quality control of diesel. Determination of cetane index, cetane number, T95, density, flash point, and viscosity in diesel can be done simultaneously in a few seconds by using the OMNIS NIR Analyzer Liquid. The possibility of fully automated analysis in combination with the OMNIS Sample Robot M – NIR increases throughput, maximizing efficiency. With the OMNIS pre-calibration of diesel (6.06008.009), users can measure all the mentioned parameters from day one.

4. Shimadzu: Analysis of Fluorine by EDXRF —A Simple Check for PFAS in Electrical and Electronic Components

• Application note
• Full PDF for download

User benefits

• EDXRF analyzes halogens (F, Cl, Br, and I) more easily than absorption/emission methods.
• Fluorine (F) on the material surface is detected directly, without sample preparation.
• Simultaneous halogen analysis enables simple screening for the possible use of halogenated flame retardants.

Asregulations on PFAS and halogenated organic flame retardants tighten in the EU1), 2) and some U.S. states3), 4), there is a growing need to identify at an early stage whether halogens such as fluorine are present in electrical and electronic materials. Rapid supply-chain screening is also increasingly required. The energy dispersive X-ray fluorescence spectrometer EDX-8100 requireslittle to no sample preparation and can quickly and easily detect halogenssuch asfluorine (F), chlorine (Cl), and bromine (Br). EDX-8100 quickly shows whether these halogens are present, helping narrow down regulated products and prioritize samples for detailed analysis. This article demonstrates the usefulness of halogen detection by EDXRF using an ETFE-coated wire and a relay as examples.

Conclusion 

As shown above, fluorine can be detected and quantified rapidly and easily when its content is about 0.1 wt% or higher. In addition to intentional use, the presence of fluorine compounds can also be confirmed in cases of unintentional inclusion,such as transfer or contamination. In the electrical and electronics field, demand for analysis related to PFAS and halogenated flame retardants is expected to increase in the future, and EDXRF is useful as a simple initial screening method