News from LabRulezICPMS Library - Week 9, 2025

Our Library never stops expanding. What are the most recent contributions to LabRulezICPMS Library in the week of 24th February 2025? Check out new documents from the field of spectroscopy/spectrometry and related techniques!

👉 SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT SPECTROSCOPY/SPECTROMETRY RELATED TECHNIQUES

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This week we bring you application notes by Agilent Technologies, Bruker, Metrohm, Shimadzu and Thermo Fisher Scientific!

1. Agilent Technologies: Sustainable Lithium-Ion Battery Recycling: Recovery of Metals in Green Solvents by ICP-OES

Fast analysis of deep eutectic solvents using Agilent 5800 VDV ICP-OES with switching valve

• Application note
• Full PDF for download

Currently, two primary industrial processes are used for recycling spent LIBs: pyrometallurgy and hydrometallurgy. Pyrometallurgy involves the high-temperature extraction of metals, which is energy demanding and yields relatively poor-quality output.³ Hydrometallurgy requires the use of numerous extractants and a longer process but achieves better metal recoveries than pyrometallurgy.³ However, the hydrometallurgical process produces large quantities of acidic and alkaline wastewater, which can threaten the environment if not properly managed.³

Deep eutectic solvents (DESs) are an emerging class of green solvents that offer a novel solution for LIB recycling. Made from mixtures of biodegradable components, DESs are easy to prepare, inexpensive, nontoxic, and reusable.⁴ Scientists are actively investigating how the unique properties of DESs can be used to efficiently leach critical metals from spent LIBs.⁴ To verify the effectiveness of DESs in terms of metal-recovery rates, researchers often use a multi-element analytical technique such as inductively coupled plasma optical emission spectroscopy (ICP-OES). However, analyzing leached metals in DESs by ICP-OES is not without its challenges. The high Total Dissolved Solids (TDS) matrix samples can cause wear on the sample introductory system, potentially introducing errors in the results. There is also a need for a wide Linear Dynamic Range (LDR), as the elemental profile of end-of-life LIBs can vary greatly.

The Agilent 5800 Vertical Dual View (VDV) ICP-OES is widely used to determine metals and other elements in LIB battery materials.⁵ Designed for robustness and stability, the 5800 enables the fast, simultaneous measurement of over 70 elements in many sample types. The wide LDR of the instrument’s Vista Chip III detector enables a range of elements to be analyzed in the same sample, avoiding the need to perform multiple dilutions.⁶ This field-proven instrument uses advanced tools and accessories to support the development of new methods, making it ideal for LIB recycling initiatives, such as facilitating the recovery of valuable metals using DESs. 

In this application, the 5800 VDV ICP-OES was used to determine eight representative elements of spent LIBs spiked in a choline chloride and urea (ChCl:Urea) DES solution. The analytes aluminum (Al), Co, copper (Cu), iron (Fe), Li, manganese (Mn), Ni, and phosphorus (P) were selected based on their presence in various types of cathode active materials (CAMs). 

Conclusion

The Agilent 5800 VDV ICP-OES with the integrated AVS 7 switching valve effectively determined valuable LIB-related elements in DES. Leaching metals from end-of-life LIBs using DESs offers a more sustainable alternative to traditional metallurgical processes for battery recycling. Under the control of Agilent ICP Expert Pro software, the 5800 enabled the fast, robust, and accurate analysis of eight representative elements of LIBs in a spiked ChCl:Urea DES solution. The following hardware and software tools were used to ensure the quality of the quantitative data:

• IntelliQuant Screening streamlined method development by recommending optimal calibration ranges and interference-free wavelengths for all analytes, ensuring accurate analysis of analytes in DESs.
• The AVS 7 improved sample throughput requiring only 41 s per sample compared to 90 s without the AVS. It also minimized costs by lowering argon consumption to 9.8 L per sample and less frequent cleaning of consumables such as the torch and nebulizer.
• FBC automatically corrected the background structures for Al, Co, Cu, Fe, Mn, Ni, and P and FACT deconvoluted the Li peak from more complex background spectra. 

The accuracy of the 5800 ICP-OES method was confirmed by recoveries of all analytes spiked at high and low levels in DES, with results within 100 ±10%. Excellent long-term stability was demonstrated when 645 solutions were analyzed over seven hours. Recoveries of the QCs and spiked DES samples were within ±10% of the expected values. Good precision was achieved for the spiked DES sample measurements, with RSDs ≤2.2% for all elements. The performance of the 5800 VDV ICP-OES with AVS 7 demonstrates its suitability for the fast, quantitative analysis of critical LIB-related elements such as Co, Mn, and Li in complex matrices like ChCl:Urea DES.

2. Bruker: Analysis of Pet Food with FT-NIR Spectroscopy

• Application note
• Full PDF for download

Pets are today an important part of peoples lives. Therefore consumers trust in brands which guarantee the best quality for their individual animal, since pets of different breed, size and age often need a special nutrient profile in their diet. Pet food producers have to provide a vast amount of different products, produced at an acceptable cost. 

From raw materials to finished pet food

The biggest challenge in pet food production is to keep track of the different recipes depending on the availability of the expensive raw materials. Depending on origin and season, they often show huge batch-to-batch variability; nevertheless, feeding the least cost formulation programs with valid compositional data is essential and a fast and accurate analysis, providing results in seconds can help keeping track of the production process.

Near infrared spectroscopy is used in agriculture for many decades for the analysis of main constituents like moisture, fat and protein. It is fast and safe, since it requires little to no sample preparation, nor hazardous chemicals or gases. This makes a quick test of the incoming raw material using FT-NIR available even to production staff, before processing the materials and also allows a fast way of testing the final material before packaging.

Easy sampling and measurement

Solid samples like like raw materials and finished pet food are filled in cups with a quartz glass bottom, placed on the integrating sphere of the MPA II or TANGO-R spectrometer and measured from below. This way, the product has an even surface and for highly reproducible results, it is rotated during the measurement. Liquid samples like oils and fats are are simply filled in 8mm glass vials and are measured in the sample compartment of the MPA II or TANGO-T.

3. Metrohm: Polyethylene content determination in polypropylene pellets by NIRS

Rapid analysis of recycled polyolefins

• Application note
• Full PDF for download

Next to polyethylene (PE), polypropylene (PP) is the most widely used plastic worldwide. Recycling these polyolefins is problematic, since it is challenging to separate polyethylene from polypropylene using sink float separation. Increasing PE content in PP leads to a poor interfacial bond strength which could negatively impact the mechanical properties of the final molded product.

An efficient method to determine the polyolefin composition based on near-infrared spectroscopy (NIRS) analysis is presented in this Application Note. The main advantage is the short time to result. Compared to the time-consuming standard method (i.e., Differential Scanning Calorimetry or DSC), the analysis of polyethylene content in polypropylene using near-infrared spectroscopy is performed in just seconds.

Experimental equipment

Different polymer blends (n = 54) with varying polyethylene content from 0.5–35% were produced in a compounder. The polyethylene content was determined by weighing before the polymer blends were produced. All measurements on the OMNIS NIR Analyzer Solid (Figure 1) were performed in rotation using a large sample cup to average the subsample spectra. This sample setup reduces the influence of the particle size distribution of the polymer particles.

Conclusion

This Application Note shows the feasibility of NIR spectroscopy for the analysis of polyolefins. Detecting PE concentrations below 5% with the standard Differential Scanning Calorimetry (DSC) method can be challenging and time consuming. Compared to DSC measurements (Table 2), near-infrared analysis saves significant time: one sample measurement is performed in a couple of seconds. Next to PE content, physical parameters like density can also be determined with NIRS. 

4. Shimadzu: Three-Point Bending Fatigue Tests of Carbon Fiber Reinforced Plastic Using the SEM Servopulser

• Application note
• Full PDF for download

User Benefits:

• The SEM Servopulser can perform three-point bending fatigue tests of carbon fiber reinforced plastic.
• The SEM Servopulser can also be used to observe fatigue cracks.
• High-accuracy dynamic control can be achieved with the Servo Controller 4830

Carbon fiber reinforced plastic (CFRP) has high specific strength and stiffness and is widely used in various industrial fields, including transport vehicles. In order to ascertain its long-term reliability and durability as a structural material, it is necessary to evaluate it for fatigue, one of the main causes of structural failure. However, since CFRP is composed of two types of materials, carbon fibers and matrix resin, it exhibits complex behaviors in failure, such as matrix cracking, inter-layer delamination,and fiber rupture.

This article describes bending fatigue tests that used the Servopulser EHF-L tabletop dynamic and fatigue testing system. The extension of cracks during the fatigue tests was observed using the SEM Servopulser, a high-temperature fatigue testing machine with a scanning electron microscope.

Conclusion

Bending fatigue tests were performed on CFRP using a fatigue testing system, and the resulting S-N curve was compiled. Then the conditions were set on the SEM Servopulser based on the SN curve obtained, and damage to the test specimen was observed during the test. By changing the magnification on the SEM, it was possible to observe the damage location on the test specimen in detail. As the test progressed, it was possible to clearly observe how the damage progressed. In this way, the SEM Servopulser demonstrated it can assist in evaluating the fatigue properties of composite materials,such as CFRP. 

5. Thermo Fisher Scientific: Measurement of traces of heavy metals in cosmetic raw materials and finished products according to ISO/DIS 21392:2021 using triple quadrupole ICP-MS

• Application note
• Full PDF for download

This application note highlights a complete and comprehensive workflow for the analysis of heavy metals in different types of cosmetic products, including raw materials, and will demonstrate the need to use triple quadrupole ICP-MS technology to achieve complete interference removal. As described in ISO/DIS 21392:2021, the samples were prepared using a microwave system prior to analysis.

Experimental

A Thermo Scientific™ iCAP™ MTX ICP-MS and a Thermo Scientific™ iSC-65 autosampler were used for analysis. The ICP-MS was operated using the parameters highlighted in Table 1. Due to the great variability of total dissolved solids (TDS) used in cosmetic matrices, the instrument was operated using Argon Gas Dilution (AGD). Thus, all calibration standards and samples were automatically diluted approximately five times to ensure analytical robustness for all sample types, such as raw materials and finished products. Due to the potential presence of interferences, the iCAP MTX ICP-MS was operated in collision (SQ-KED) and reaction (TQ-O2) modes to remove polyatomic and isobaric interferences, and to reach the best quantification limits for critical elements.

Conclusion

As the demand for cosmetic products continues to grow worldwide, the testing of raw materials and finished cosmetic products becomes a key activity to ensure consumer safety with respect to exposure to potentially toxic heavy metals. Maintaining stringent safety standards remains a priority to protect consumer health and uphold the reputation of the industry. The proposed method provides a powerful and reliable option for both manufacturers as well as testing laboratories to obtain high quality data in combination with the often-required productivity. It ensures regulatory compliance with ISO/DIS 21392:2021, but also provides valuable insights as also other elements, currently not under regulation, can be determined free from interferences and potential biases.

Some key advantages are summarized below:

• The automated sample preparation with the combination of the EasyFILL Acid Delivery and the ultraWAVE SRC microwave system ensures an efficient and reproducible method for the acid digestion of the cosmetic samples.
• EasyAGD delivers a constant and automatic 5-times dilution for all samples, which allows laboratories to analyze finished products as well as raw materials in the same batch with excellent robustness.
• The use of the iCAP MTX ICP-MS allows the leveraging of oxygen as a reactive gas in TQ-O2 mode to overcome critical interferences and to obtain the lower quantification limits required by the regulation for highly toxic heavy metals.
• The presence of high concentrations of tungsten, tin, and zirconium in certain raw materials can create isobaric and polyatomic interferences on toxic heavy metals such as mercury and cadmium. The use of TQ-O2 mode guarantees excellent method accuracy for all sample types.
• Workflows can be further streamlined using innovative features such as the Get Ready process for automatic and scheduled plasma start. The Thermo Scientific™ Hawk™ Consumables and Maintenance Assistant within Qtegra ISDS Software allows contract testing laboratories to ensure all maintenance activities are accomplished before unexpected downtime of the system impacts laboratory productivity.