News from LabRulezICPMS Library - Week 40, 2024

Our Library never stops expanding. What are the most recent contributions to LabRulezICPMS Library in week 40, 2024? Check out new documents from the field of spectroscopy, especially ICP/MS techniques!

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This week we bring to you applications by Agilent Technologies, Shimadzu, and Metrohm and a poster by Thermo Fisher Scientific!

1. Agilent Technologies: Reducing Instrument Downtime in Elemental Analysis of Lubricant Oils as per ASTM 5185

• Application

Run samples faster and for longer using the V-groove nebulizer

Abstract

In this application note, lubricant oil samples were analyzed using an Agilent 5900 Synchronous Vertical Dual View (SVDV) inductively coupled plasma optical emission spectrometer (ICP-OES) coupled with an Agilent Advanced Valve System 6 (AVS 6) and the Agilent V-groove nebulizer to enable the rapid analysis of over 1,000 samples in 6 hours (more than 160 samples per hour). The V-groove nebulizer provides exceptional performance characteristics, robustness, and durability, even when using troublesome samples. It also provides a reduction in sample loading on the plasma, which reduces carbon formation on the injector of the torch, allowing extended run times, while exceeding the sensitivity requirements required for the ASTM D5185-18 standard method.

Introduction

Elemental analysis of lubricant and hydraulic oils is essential for predictive and preventive maintenance, as well as trend analysis in many heavy industries. The ASTM D5185‑18 standard method1 is the gold standard in tribology laboratories globally to quantify additive elements, wear metals, and contaminants. This method uses ICP-OES for the rapid elemental determination of 22 elements in both used and unused lubricating and base oils, providing quick screening of used oils for signs of wear.

Tribology laboratories typically process hundreds of samples daily; therefore, they are constantly searching for ways to enhance efficiency and improve sample throughput. Instrument downtime caused by blockages in the sample introduction system (SIS) can be a common problem in these high-throughput labs. These blockages are typically caused by suspended particles in the samples blocking the nebulizer, and carbon deposits blocking the injector of the torch. Although various methods exist to remove the blockage from the nebulizer and clean the torch, all require extinguishing the plasma to remove and clean the SIS.

The use of a robust nebulizer is a strategy that can enable tribology laboratories to run more samples with reduced blockage. This will improve their workflows and increase sample throughput, reducing both instrument downtime and their running costs. One example of a robust nebulizer that helps to overcome the blockage issues is the inert, high-total-dissolved-solids (high-TDS) Agilent V-groove nebulizer, which is capable of aspirating highly dissolved solids and slurries (up to 30% dissolved solids with a maximum particle size of 350 μm). Its inert construction also ensures that any solvent can be nebulized.

In this application note, used diesel engine lubricant oil samples were analyzed using the 5900 SVDV ICP-OES coupled with the AVS 6 and the V-groove nebulizer, following the ASTM D5185-18 standard method. 

Conclusion

This application note shows the suitability of the Agilent 5900 SVDV ICP-OES used with the Agilent AVS 6 and inert V-groove nebulizer for rapid multi-element analysis of used lubricant oil samples using the ASTM D5185-18 standard method.

Excellent long-term stability was demonstrated when more than 1,000 samples were analyzed over a six-hour period (22 to 23 seconds per sample). All measurements of this spiked oil sample were within ± 10% of the expected value, with precision better than 5% RSD in most cases. The spike recovery study showed how the 5900 ICP-OES, used with the inert V-groove nebulizer, can accurately detect low range concentrations of wear metals and high concentrations of the elements from the additive package in a single analysis. The inert V-groove nebulizer also enabled the samples to be run faster, with excellent accuracy.

Despite no oxygen injection being used, there were no signs of blockage of the injector of the torch, or carbon deposition after the test. The V-groove nebulizer design reduces sample loading on the plasma, minimizing carbon buildup while maintaining the sensitivity required for the ASTM D5185 standard method. No nebulizer blockage was experienced while collecting the data for this study. The inert V-groove nebulizer allows extended run times by reducing the frequency of torch and nebulizer maintenance. This demonstrates the stability of the 5900 ICP-OES and the suitability of the inert V-groove nebulizer for high-throughput tribology laboratories, by reducing instrument maintenance downtime and improving sample throughput.

2. Thermo Fisher Scientific: WPC: Sensitive and interference free analysis of halogens using triple quadrupole ICP-MS

• Poster / WPC

ABSTRACT

The analysis of halogens is important in many different industries, such as environmental monitoring, pharmaceutical, oil and gas, but also Li-ion battery and renewable fuels. Halogen analysis is commonly carried out using ion chromatography (IC), whereas argon plasma-based techniques like ICP-MS are less common, due to poor sensitivitiy, and potential spectral interferences. This study describes a complete analytical workflow using the Thermo Scientific™ iCAP™ TQe ICP-MS for the accurate and precise quantification of challenging halogen analytes like fluorine, chlorine, and bromine.

CONCLUSIONS

This work highlights how triple quadrupole ICP-MS systems, such as the iCAP TQe ICP-MS, operated in TQ-O 2 mode can be used for accurate and precise quantification of challenging analytes such as halogens.

• It could be shown that chlorine and bromine can be analyzed directly using optimized instrument conditions.
• It further highlights the feasibility of iCAP TQe ICP-MS for indirect but accurate and precise determination of fluorine by following approach of complex formation with barium under optimized and controlled conditions
• The analytical data and observations made during this study strongly suggest that iCAP TQe ICP-MS equipped with dedicated mass flow controllers (MFCs) for introduction of pure oxygen and pure helium as cell gases is a powerful tool to accomplish the otherwise challenging analysis of halogens.
• Upcoming studies will focus on the application of the fluorine measurements in hyphenated techniques, such as liquid chromatography hyphenated to ICP-MS to assess the potential for emerging contaminant screening, i.e. of PFAS

3. Shimadzu: Analysis of Elemental Impurities in Anode Materials for Lithium-Ion Secondary Batteries Using the ICPE- 9820

• Application

User Benefits

• Elemental impurities in the anode materials of lithium-ion secondary batteries can be measured.
• Even after measurement, elements and wavelengths can be added to check for unexpected elemental impurities in the anode materials.
• The system uses a mini torch that consumes less argon gas, thus reducing running costs.

Introduction

Lithium-ion secondary batteries (LIBs) are widely used in mobile devices, electric vehicles, hybrid cars, and more. One of the components of LIBs, the anode, accumulates and releases Li ions during charging and discharging. Graphite-based materials are mainly used as the anode material in LIBs. In China, one of the major producers, the analysis of elemental impurities in graphite, which is used as LIB anode material, is required by GB/T 24533-20191) using inductively coupled plasma atomic emission spectroscopy (ICP-AES).

In this Application News, elemental impurities in LIB anode materials were analyzed using the ICPE-9820. Spike recovery tests were performed to confirm the validity of the analytical values. Additionally, the “Acquisition for All Wavelength” feature allows for checking the presence of elemental impurities that were not subjected to quantitative analysis.

Conclusion

In this Application News, an analysis of elemental impurities in LIB anode materials was performed using the ICPE-9820. Good spike recoveries were obtained, confirming the accuracy of the analysis. Additionally, elements and wavelengths were added after the measurement to identify elemental impurities other than the analyzed elements present in the anode materials.

4. Metrohm: Monitoring complexing agents in galvanic baths inline with Raman spectroscopy

• Application

The main purposes of galvanic process baths include the surface refinement of workpieces and the setting of physical properties. To this end, bath additives (e.g., organic compounds or complexing agents) are regularly added in different amounts, depending on the processing load. Since the bath composition changes continuously due to the introduction of the workpieces, close monitoring of the concentration of the bath additives is necessary to ensure that the end product quality is at the highest level.

This Process Application Note presents a method to accurately analyze complexing agents inline in galvanic baths with a 2060 Raman Analyzer from Metrohm Process Analytics. This enables real-time bath control and thus an increase in production efficiency and product quality.

CONCLUSION

Raman spectroscopy is an easy-to-use analytical technique that identifies liquids and solids within seconds. The 2060 Raman Analyzer from Metrohm Process Analytics is a high-performance Raman system designed for monitoring different processes like electroplating.

Together with Metrohm’s Vision and IMPACT software, the 2060 Raman Analyzer can be used to acquire real-time results, increase roductivity, and lower production costs.