News from LabRulezICPMS Library - Week 11, 2025

Our Library never stops expanding. What are the most recent contributions to LabRulezICPMS Library in the week of 10th March 2025? Check out new documents from the field of spectroscopy/spectrometry and related techniques!

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This week we bring you application notes by Agilent Technologies, Bruker and Shimadzu and brochure by Anton Paar!

1. Agilent Technologies: Method Verification of the United States Pharmacopeia Monograph with the Agilent Cary 60 UV-Vis

Quantification of iron impurities in magnesium sulfate following the USP monograph 

• Application note
• Full PDF for download

Government agencies at national and international levels regulate pharmaceuticals to ensure the safety, efficacy, quality, and labeling of drugs. These agencies publish pharmaceutical monographs for drug developers and manufacturers, helping them to maintain consistent quality standards throughout the research, development, and manufacturing processes. Major pharmacopoeias, such as the USP, European Pharmacopoeia (Ph. Eur.), British Pharmacopoeia (BP), Japanese Pharmacopoeia (JP), and Pharmacopoeia of the People's Republic of China (ChP) publish pharmaceutical monographs as part of their official compendia. Monographs provide methods for the quantitative determination of pharmaceutical substances, including the measurement of impurities within acceptable limits, and are essential for compliance with regulatory requirements. UV-Vis spectroscopy is a commonly specified technique in various pharmaceutical monographs. 

According to good manufacturing practices (GMP), any techniques that are used to analyze pharmaceutical substances must be evaluated to determine their suitability under actual conditions of use. The USP provides general information on the verification of compendial procedures in USP General Chapter <1226> Verification of Compendial Procedures and specific guidance on UV-Vis spectroscopic techniques in USP General Chapter <857> Ultraviolet-Visible Spectroscopy.^1,2 

In a previous application note, the Cary 60 UV Vis spectrophotometer and Cary WinUV software performed the measurements that are required by many of the verification tests outlined in USP <857>.³ This study provides an example of how the Cary 60 UV-Vis fitted with an 18-cell multicell changer can be used for method verification for the quantification of iron in magnesium sulfate per the USP Magnesium Sulfate monograph.⁴

Conclusion 

An Agilent Cary 60 UV-Vis with an 18-cell changer was used to demonstrate how a UV-Vis compendial procedure from a USP monograph can be verified. The Agilent Cary WinUV software and 18-cell changer automated the multiple replicate measurements required by the USP validation tests, reducing the workload of the operator. The validation tests included confirmation of measurement accuracy, precision, specificity, and determination of the quantitation limit. 

After verifying the method, the Cary 60 UV-Vis was used to measure the content of iron in two magnesium sulfate samples following the USP Magnesium Sulfate compendial procedure. The results were within the acceptance criteria for that material of < 0.5 μg/g. 

The Cary 60 UV-Vis is ideal for routine pharma quality assurance/quality control (QA/QC) workflows and R&D applications. Optional Agilent Cary WinUV Pharma software is also available that supports compliance with US FDA 21 CFR Part 11, EU Annex 11, and similar national electronic record regulations.

2. Anton Paar: Microwave Digestion Platform - Multiwave 5001 | Multiwave 3001

• Brochure
• Full PDF for download

Even the most advanced analytical equipment delivers inconsistent measurement values without precise and flawless sample preparation. That’s where Anton Paar’s Multiwave 5001 and Multiwave 3001 come in. We’ve channeled over 50 years of sample preparation expertise into a microwave system that fits every need. From routine samples to highly demanding ones, and for every kind of throughput or application need, Multiwave 5001 and Multiwave 3001 are the answer. You’ll be equipped to handle every complex testing requirement you may have.

• Premium digestion parameters: Up to 300 °C and 100 bar 
• Powerful: Saves time, boosts throughput, and reduces costs, with up to 64 samples in a single run 
• Intelligent: 600 pre-installed programs, guiding features, tool-free vessel handling, and a “clever” door 
• Connected 24/7: Automated data export for optimally traceable results 
• Safety: Independent certification of safety features ensures they are at the highest level 
• AP Connect: Can be integrated with our lab execution software AP Connect

Multiware 5001 (One instrument, every application)

Some samples require special treatment. Multiwave 5001 provides premium digestion parameters and many additional sample preparation methods. This instrument combines more than 50 years experience in sample preparation with state-of-the-art technology.

• Full variety of applications and vessels – up to 300 °C and 100 bar
• Advanced sensor technology (SmartTemp 2.0)
• AP Connect (lab execution software) and automated data export
• Optional digital camera inside the chamber

Further applications for Multiwave 5001 

Extraction 

The perfect alternative to conventional methods thanks to reduced reaction times and solvent consumption. A costeffective way to improve the performance and throughput of HPLC- or GC-based analysis routines. Multiwave 5001 is suitable for extractions of PCBs, PAHs and hydrocarbons, derivatization reactions prior to analysis, and polymer extractions. 

Evaporation 

The 24EVAP accessory facilitates the evaporation of acids and concentration of aqueous sample solutions even without the need to transfer digestion solutions. It offers automatic endpoint determination for a variety of samples. The external scrubber neutralizes the acid vapors with a washing efficiency of more than 95 %. 

Drying 

Rotor 1DRY efficiently dries samples 4x faster than conventional methods, and provides samples without carbonization or contamination. Humidity and unwanted odors are removed via the exhaust system. 

Microwave-induced oxygen combustion (MIC) 

This unique, clean, and quick method is suitable for all combustible solids (wood, paper, coal, food, or polymers). Analytes are trapped in a low-concentration absorption solution which can be measured without dilution.

Multiware 3001 (High throughput at affordable costs)

Routine samples require robust workflows at minimum effort and cost per sample. Multiwave 3001 is the instrument with the best performance-to-cost ratio, digesting up to 41 samples in a single run. Benefit from proven features including SmartVent technology and a comprehensive method library.

• Efficient digestion of routine samples, with HVT vessels
• Reliable temperature measurement thanks to robust IR method
• Automated data export

3. Bruker Optics: Used Lubcricating Oil Analysis by FT-IR:
An Overview

• Application note
• Full PDF for download

Oil analysis by FT-IR is a simple method to detect dilution, degredation or illegal additives in all types of oils. 

Fourier-Transform Infrared spectroscopy utilizes the interaction of invisible infrared radiation and matter. This yields valuable molecular information and allows the identification of chemicals in a few seconds without consumables or additional chemicals. Generally, this can be used on solids, liquids and gases and of course industrial oils. This method has been widely accepted and is used by automotive industries, drilling companies, legal authorities and even at F1-racing events.

Why are in-service lubricating oils tested? 

To readily assess the lubricant’s performance, testing and diagnosis of oils in-service is necessary. This is especially important to prolong engine life and avoid sudden and unforeseen damages to the engine. Lubricating oils reduce friction and protect the engine’s moving parts from wear and corrosion. In diesel engines, the oil must also suspend soot particle resulting from incomplete fuel combustion to avoid depositions. 

If the lubricant is saturated, performance decreases significantly. The analysis of in-service oils also provides information about engine-related functions to identify component failures or harmful operating conditions. 

Advantages of FT-IR in oil analysis 

For one, the low cost of modern Fourier transform (FT-IR) systems, along with the ability to obtain high-quality data rapidly has made this technique very attractive. Especially in routine analysis, there is a strong demand for for quick results in routine monitoring of in-service lubricant. FT-IR has already started to gradually replace replace various time-consuming and tedious traditional wet chemical and physical analysis methods. 

Therefore, the ASTM adopted a standard practice E2412 titled; “Standard Practice for Condition Monitoring of Used Lubricants by Trend Analysis Using Fourier-Transform Infrared (FT-IR) Spectrometry” illustrating the increased application of FT-IR spectroscopy in this field.

Conclusion 

FT-IR is a reliable and valid approach to oil analysis, that not only allows you to access a lot of information with a single measurement, but also simplifies the procedure. Infrared spectrometers come in various shapes and configurations and Bruker even offers a dedicated used oil analysis kit.

4. Shimadzu: Major Component and Elemental Impurity Analysis of Lithium-Ion Cathode Materials Using the ICPE-9820

• Application note
• Full PDF for download

User Benefits:

• The system uses a mini torch that consumes less argon, thus reducing running costs.
• Measurements are stable with minimum long-term and daily fluctuations.
• Post-measurement addition of elements and wavelengths is simple, enabling quantification at optimal wavelengths without remeasurement.

Lithium-ion secondary batteries (LIBs) are used in many products, such as smartphones and electric vehicles, because they are small and lightweight yet offer high capacity or energy density. However, there is a risk of ignition and heat generation, makes ensuring safety a critical issue. The elemental composition of cathode materials is known to be one of the most important factors that affect energy density and safety. In this Application News, the main elements and impurity elements of LIBs cathode material were analyzed using the ICPE9820 (Fig. 1). Validation tests on the analysis values and stability tests (2.5 hours variation, 5 days daily variation) on the main components were performed.

Analysis Wavelength of Elemental Impurity Analysis

The wavelength recommended by the ICPEsolution software as the analysis wavelength was chosen. ICPEsolution enables users to identify recommended wavelengths that have a low background equivalent concentration (BEC) and are generally less susceptible to interference from the wavelengths registered for each element (Fig. 5). The sample for elemental impurity analysis was analyzed with the calibration standards shown in Table 6. 

Since the cathode materials contain a large amount of Li, Co, Ni, and Mn, spectroscopic interference from these major elements may occur during the analysis of elemental impurities. Therefore, it is important to select the optimal wavelength, one that is unaffected by spectral interference. 

The 202.548 nm and 213.856 nm wavelengths of Zn have high sensitivity with low BEC (Fig. 5), but the peaks of Ni and Co overlap at 202.548 nm, and the peaks of Ni overlap at 213.856 nm (Fig. 6). 

As shown in Fig. 5, ICPEsolution allows users to check which element peaks are likely to overlap using the “Peak Search” function. In addition, the “All-wavelength Data Acquisition” function allows data readout after measurement. Even if the major components are unknown, qualitative analysis of all elements can be added after the measurement, and it is easy to determine which elements are contained in large amounts. Using this function, users can confirm and quantify the profile of a wavelength that has not been registered without needing to re-measure. In this study, 206.200 nm, which is free from interference, was used for quantitative analysis of Zn (Fig. 7). S has relatively low BEC at 180.731 nm and 182.037 nm, but Mn interferes with both. At 182.625 nm, there is slight B interference B, but since it was confirmed that the concentration of B in the sample was below the detection limit, 182.625 nm was used. 

If the sample contains a large amount of B, it is better to perform inter-element correction at 180.731 nm, where the Mn interference is relatively small. With ICPEsolution, the user can easily perform inter-element correction by simply selecting the elements and wavelengths to be used for the operation. Care must be taken in cases where the correction amount is much larger than the quantitative value of S since an error is likely to occur (Fig. 8).

Conclusion 

In this Application News, the ICPE-9820 was used to analyze the major components and elemental impurities in LIBs cathode materials. Analysis of the major components showed that the results were stable over long periods and showed little day-to-day variation. Good results were obtained in the analysis of elemental impurities in spike recovery tests, and the validity of the analysis was confirmed. In addition, elements and wavelengths were added after the measurement, and it was possible to determine the appropriate analytical wavelength without re-measurement. The ICPE-9820 offers both low running costs and stable measurements. In addition, convenient functions such as the acquisition of all wavelength data make it possible to efficiently analyze even samples with high spectral interference. Therefore, the ICPE-9820 is the ideal instrument for elemental analysis of LIBs cathode materials.