News from LabRulezICPMS Library - Week 46, 2025

Our Library never stops expanding. What are the most recent contributions to LabRulezICPMS Library in the week of 10th November 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 LECO and Shimadzu and poster by Thermo Fisher Scientific!

1. LECO: Compositional Depth Profile Analysis of Galvanized Steel

• Application note
• Full PDF for download

• Thickness and Coating Weight of Galvanized Steel 
• Elemental Composition of the Coating and Substrate 
• Compositional Analysis of Surface Treatments

The application of zinc and zinc-alloy coatings to steel provides protection against galvanic and barrier corrosion. Galvanized coatings can be applied by either continuous hot-dip coating or electroplating. Hot-dip coatings include galvanized (zinc), galvannealed, and 55% aluminum-zinc. Electroplated coatings include zinc and zinc-nickel. The choice of coating depends on the application. Thin coatings provide sufficient corrosion resistance where the corrosion rate is low, such as interior panels and painted parts. Thick coatings are needed where corrosion rate is high and long service life is required, such as marine or underground applications.

Compositional Depth Profile (CDP) using the LECO GDS950 rapidly provides analysis of various galvanized coatings on steel. The analyses shown in this Application Note conforms to and is in accordance with ISO 16962.

Conclusion 

As demonstrated in this application note, CDP analysis on the LECO GDS950 provides coating composition as a function of depth for a variety of galvanized coatings, including both conductive and non-conductive coatings. Most zinc coatings can be analyzed in 60-300 s. The 55% aluminum-zinc alloy sputters more slowly and can be analyzed in 600-900 s. CDP using the LECO GDS950 provides a single flexible method to analyze multiple zinc and zinc-alloy coating types.

2. Shimadzu: Determination of Water-Extractable Total Organic Carbon Content in Recycled Black Mass

• Application note
• Full PDF for download

User Benefits

•  Measurement of the water-extractable TOC content in recycled black mass is possible.
• Using the NPOC method, TOC measurement can be simplified thanks to reduced preprocessing.
• Utilizing the ASI-L auto sampler enables multiple samples to be measured automatically

Black mass is a concentrated powder created during the recycling of lithium-ion batteries. It contains valuable metals such as cobalt and nickel, which are cathode active materials, as well as graphite, which is an anode active material. Since black mass contains these valuable metals, its recycling and reuse significantly contribute to reducing environmental impact and promoting the efficient utilization of resources. 

Black mass may contain organic substances derived from used batteriesthat serve asraw materials, as well as organic substances from the environmental sources introduced during storage and transportation. These organic substances can leach into water or acidic solutions, which may adversely affect the refining process. This not only results in poor-quality recycled materials but also leavesresidual organic substancesin the waste liquids, potentially causing environmental pollution. Therefore, it is essential to quantify the total amount of organic substances contained in black mass. The amount of these organic substances can be evaluated astotal organic carbon (TOC). 

In China, one of the major importing countries of black mass, the evaluation of water-extractable TOC in black mass is regulated under the Chinese National Standard GB/T 45203- 2024. 1) According to this standard, TOC is measured using a total organic carbon analyzer based on the combustion oxidation method with non-dispersive infrared (NDIR) detection. This article provides an example of measuring water-extractable TOC in black mass using the Shimadzu TOC-L analyzer, a total organic carbon analyzer that uses the combustion oxidation method with NDIR detection.

TOC Analysis Using the NPOC Method 

In the NPOC method, the sample is acidified by adding acid, and IC is removed through aeration treatment. The measurement is then performed under the assumption that “TC = TOC.” In the NPOC method, the instrument automatically performed acidification and aeration. This method is expected to reduce measurement time compared to the TC-IC method, and only a single calibration curve isrequired. 

Fig. 4 illustrates the pretreatment flow when using the NPOC method. Here, IC in the solution can be efficiently removed through automatic acidification and aeration by the instrument. As a result, Step 3, “Acidification and Aeration Treatment,” in the pretreatment procedure can be omitted. A 5 mL aliquot of the filtrate obtained in Step 2, “Filtration,” was directly diluted to 100 mL in a volumetric flask, and the resulting solution was used as the measurement solution. 

When no acidification is performed during pretreatment, the measurement solution becomes alkaline. Therefore, in the NPOC measurement, the acid addition rate was set to a relatively high value of 2.5 %. 

The NPOC method is not described in GB/T 45203-2024; however, it is expected to improve processing efficiency by simplifying manual procedures.

Conclusion 

In this study, the water-extractable TOC in recycled black mass was determined using the Shimadzu TOC-L total organic carbon analyzer that uses the combustion oxidation method with NDIR detection. Pretreatment was performed with reference to GB/T 45203- 2024, and it was confirmed that the water-extractable TOC in black mass could be measured using the TC-IC method. 

On the other hand, by using the NPOC method, certain pretreatment steps could be omitted, enabling a more simplified quantification of TOC. This method is effective for improving measurement efficiency in applications such as screening. In both measurement methods, satisfactory results were obtained in the spiked recovery tests, confirming the validity of the analysis. Furthermore, by utilizing the ASI-L auto-sampler, multiple samples can be measured automatically, contributing to improved analytical efficiency.

3. Thermo Fisher Scientific: Do we have a choice of reaction gas for measuring Ca? Investigations using the Thermo Scientific Neoma MS/MS MC-ICP-MS

• Poster
• Full PDF for download

Calcium isotope measurements have long been limited by isobaric interferences, particularly from ⁴⁰Ar⁺ on ⁴⁰Ca⁺, when using multi-collector inductively coupled plasma mass spectrometry (MC-ICP-MS). The reintroduction of collision/reaction cell technology to MC-ICP-MS systems, such as the Thermo Scientific Neoma MS/MS MC-ICP-MS, has allowed more precise δ⁴⁴/⁴⁰Ca determinations using hydrogen (H₂) as a reaction gas. However, researchers investigated whether sulfur hexafluoride (SF₆) could offer an alternative, forming CaF⁺ and removing both ⁴⁰Ar⁺ and ⁸⁸Sr²⁺ interferences, thereby simplifying sample preparation and enabling in-situ Ca isotope analysis by laser ablation.

Experimental

Measurements were performed on the Thermo Scientific Neoma MS/MS MC-ICP-MS equipped with three 10¹³ Ω amplifiers and an axial secondary electron multiplier. The Jet interface with X-skimmer and Jet sampler cones, and an ESI Apex Omega Q desolvating nebulizer, were used to maximize sensitivity. Reaction gases—helium and SF₆—were introduced into the collision/reaction cell. Both solution and solid samples (analyzed by coupling the Neoma MS/MS to an ESL NWR imageGEO 193 nm excimer laser ablation system) were tested. Solid samples included reference glasses (SRM 614, BHVO-2G) and apatites (Durango, Madagascar, SUME, iPiRA). Data reduction was done using Iolite 4 software with a custom CaF⁺ reduction scheme.

Results

Using SF₆ as the reaction gas effectively formed CaF⁺ ions, reducing argon and strontium interferences. However, sensitivity decreased about five-fold compared to the H₂/He setup, and molecular interferences—likely ³²S¹⁹F¹⁴N⁺ and ³²S¹⁹F¹⁶O⁺—affected minor isotopes (⁴⁶Ca, ⁴⁸Ca). Reproducibility of ⁴⁰Ca/⁴⁴Ca was poorer than that of ⁴²Ca/⁴⁴Ca and ⁴³Ca/⁴⁴Ca despite higher ⁴⁰Ca sensitivity. For most solution and solid standards, δ⁴²Ca and δ⁴³Ca values matched expected ranges. Solid-state tests via laser ablation showed generally consistent isotopic ratios, with slightly higher uncertainty for low-Ca materials.

Conclusion

The study demonstrated that SF₆ can be used as a viable reaction gas for interference-free measurement of Ca isotopes on the Neoma MS/MS MC-ICP-MS, offering potential for in-situ analysis and reduced sample preparation. However, H₂ remains the superior choice for solution-based analyses due to its higher sensitivity, better precision, and fewer molecular interferences. SF₆, on the other hand, provides a promising alternative for direct solid-sample applications, such as laser ablation Ca isotope ratio studies.