News from LabRulezICPMS Library - Week 2, 2025

Our Library never stops expanding. What are the most recent contributions to LabRulezICPMS Library in the week of 6th January 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 applications by ALS Europe, Thermo Fisher Scientific, Agilent Technologies and Shimadzu!

1. ALS Europe: Precision and Detail Ensured by Scanning Electron Microscopy

• Technical note
• Full PDF for download

A Scanning Electron Microscope equipped with Energy-Dispersive X-ray Spectroscopy (SEM-EDS) represents a powerful tool and robust analytical technique that offers an extensive array of data regarding the microstructural and compositional attributes of a diverse spectrum of materials. ALS Laboratories are equipped with a modern scanning electron microscope Tescan VEGA 3 LMU with an energy-dispersive detector (EDS) Oxford X-Max 20. It is an ideal technique for surface inspection, identification of the elemental composition of unknown particles in a sample, or advanced determination of particle size or type distribution.

Elemental Analysis

An effective complement to the microscope itself is the aforementioned EDS detector, which can detect characteristic X-rays and assign them to specific elements. The latest systems are capable of detecting elements heavier than boron, i.e., elements with an atomic number >5. The Oxford AZtec X-Max 20 EDS detector in our laboratories can very quickly confirm or exclude the presence of elements heavier than beryllium (excluding hydrogen, helium, and lithium). The result is a spectrum from which the composition of the examined particle can be determined. This capability can be utilised, for example, to compare the sample material with a supplied standard or to observe changes occurring in the sample when exposed to various processes and conditions.

Feature Analysis

Using the software module "Feature Analysis," it is possible to automatically analyse a large number of particles in terms of morphology, chemical composition, or a combination of both. A significant advantage over common techniques such as laser diffraction is the ability to directly image the analysed particles. The particles can be sorted entirely automatically, either by morphology, by defining parameters such as length, area, shape, etc., or by chemical composition, for example, whether they contain a specific element or not. The outputs can include various graphs and tables (see Figures 4 (A/B).

The most common analyses in ALS Laboratories include: the anti-corrosion coating of car parts, the specification of foreign particles, a very frequent analysis is an identification of deposits on filters, identification of sediments, or stains, and defects on the surface of various materials and products. SEM-EDS analysis is also often an integral part of production processes, where quality control of intermediate and final products is crucial.

2. Thermo Fisher Scientific: Analysis of photovoltaic grade silicon using triple quadrupole inductively coupled plasma mass spectrometry (ICP-MS)

• Application
• Full PDF for download

To demonstrate a robust and accurate analytical method for the determination of bulk and trace elements in photovoltaic samples using triple quadrupole ICP-MS

Introduction

Development of renewable and low-carbon energy sources has become critical in addressing global concerns related to carbon emissions and climate change. One key technology in achieving the reduction of CO₂ emissions while ensuring a stable and reliable energy supply is the use of photovoltaic (PV) technology. PV technology harnesses the natural energy from the sun and converts it into electrical power, emits zero CO₂, and enhances energy security. Additionally, PV solar cells are predominantly composed of silicon, an abundant resource on Earth, making the transition to PV energy a viable option as a primary source of electricity, aligning with the move towards climate-friendly energy resources.

However, it is important to acknowledge that PV also has certain drawbacks, including susceptibility to damage, dependence on sunlight, and associated costs. To address these concerns, it is crucial to focus on developing innovative solutions that result in durable products, increased energy efficiency, and degradation prevention.

Experimental optimization of the instrument parameters

An iCAP MTX ICP-MS, operated together with a Thermo Scientific™ iSC-65 Autosampler, was used for all analyses. The sample introduction system consisted of a Peltier-cooled (at 2.7 °C) and dedicated HF sample introduction kit consisting of a baffled PFA cyclonic spray chamber (Savillex, Eden Prairie, MN, USA), PFA concentric nebulizer (Savillex), and PLUS torch1 with a 2.0 mm i.d. removable sapphire injector. The built-in argon humidifier was used for moisturizing the nebulizer gas to prevent salt deposit on the
nebulizer tip, along with integrated argon gas dilution. 

To further increase uptime of the instrument, intelligent matrix handling was used, a unique feature of the Thermo Scientific™ iCAP™ MX Series ICP-MS instruments to reduce exposure to sample matrix during sample uptake and wash. Interferences on all analytes were effectively controlled using the QCell collision/reaction cell (CRC) and leveraging the superior interference removal capabilities of a triple quadrupole ICP-MS instrument. In addition to the use of O₂ as a reactive gas in triple quadrupole mode for highly interfered analytes such as phosphorus, sulfur, arsenic and selenium, the instrument was also operated in single quadrupole mode using helium and kinetic energy discrimination (KED) for interference free analysis of other analytes over the full mass range. Table 1 summarizes the instrument configuration and analytical parameters.

The selection of the most appropriate isotopes per analyte, as well as the optimum analysis conditions (i.e., KED mode versus reactive gas, on mass mode versus mass shift mode) was automatically accomplished using the Reaction Finder Method Development Assistant available in the Thermo Scientific™ Qtegra™ Intelligent Scientific Data Solution™ (ISDS) Software. Measurement modes were optimized using the provided autotune procedures.

The iSC-65 Autosampler allowed for the use of Step Ahead functionality to shorten the overall measurement time per sample and increase the number of samples that can be analyzed per unit time.

3. Agilent Technologies: ICP-OES Analysis of Electrolytes for All-Vanadium Redox Flow Batteries

• Application
• Full PDF for download

Quantification of impurity elements in vanadium sulfate electrolytes using an Agilent 5800 VDV ICP-OES.

The detrimental effects of burning fossil fuels on the climate, environment, and air quality are driving the shift towards cleaner and more sustainable sources of energy. However, challenges remain for the renewable energy sector, as both wind and solar power can be intermittent, leading to fluctuations in energy generation. To offset the uncontrollable nature of these weather-based technologies, there is increasing demand for large-scale energy storage solutions to balance the requirements of energy grids. Addressing these challenges is crucial for achieving sustainable, reliable, and secure systems that can meet both current and future energy needs.

Compared to traditional batteries, which store energy in the electrodes, flow batteries are electrochemical (redox) systems that store and release energy through chemical reactions within the electrolyte. This mechanism means that the capacity and power of flow batteries can be tailored separately, providing scalability and long lifespans. This flexibility makes them suitable for grid-scale energy storage and backup power systems.

Instrumentation

Elemental analysis of the samples was carried out using the Agilent 5800 VDV ICP-OES. The instrument was fitted with a SeaSpray glass concentric nebulizer, double-pass cyclonic spray chamber, and an Easy-fit fully demountable torch with 1.8 mm quartz injector.

Agilent ICP Expert software was used to control the 5800 ICP-OES, optimize and run the method, and to process the data.

Automatic background correction

The Fitted Background Correction (FBC) routine within the ICP Expert software was used for all elements in this study. FBC uses a sophisticated mathematical algorithm to automatically model and subtract simple and complex background structures produced by non-analyte signals.

Conclusion

The Agilent 5800 VDV ICP-OES successfully determined 11 impurity elements in four all-vanadium flow battery electrolytes—an important quality control application within the battery production process. The main advantages of the analytical method include:

• Good calibration linearity (R>0.9999) and low method detection limits (<0.09 mg/L) for all target analytes.
• Confirmation of the method’s accuracy demonstrated by 94 to 103% recoveries of 0.5 mg/L spikes added to one of the commercial vanadium sulfate electrolyte samples.
• Recovery of all elements within 100 ±10% indicating that the 5800 can tolerate the high concentration of vanadium in the electrolyte samples, due to its robust vertical plasma and SSRF generator.
• Excellent instrument stability, as shown by the precision of repeated measurements of a commercial electrolyte sample over four hours (RSDs < 2.3%).

The 5800 VDV ICP-OES method is suitable for the accurate quantification of some key impurity elements in electrolytes used in all-vanadium flow batteries, in accordance with China standard method GB/T 37204-2018.

4. Shimadzu: Observation of Rubber Fatigue Testing Specimens Using Two Types of X-Ray CT Systems

• Application
• Full PDF for download

User Benefits

• The volume and shape of individual micro-defects in rubber can be observed in detail using a microfocus X-ray CT system.
• The approximate position and size of microcracks can be determined efficiently using a phase-contrast X-ray CT system.
• The progression status of defects and cracks in rubber can be compared at respective cycle counts of fatigue testing.

Rubber products serve an important role in a wide range of fields, such as automotive tires, industrial products, and medical devices. However, functional losses can occur due to fatigue and aging after long periods of use. Therefore, evaluating the durability of rubber is an important issue.

In order to evaluate the progression of defects during usage, rubber must be inspected before it fails. It can be inspected by cutting it apart, but non-destructive inspections are preferable due to the disadvantages of destructive inspections, such as the inability to restore specimens after inspections and the limitation of only being able to evaluate cut surfaces.

Internal defects can be detected and three-dimensionally observed using an X-ray CT system. One X-ray imaging method typically used is absorption imaging, which generates images based on the quantity of X-rays absorbed. Another method is phase imaging, which is a new unconventional method that generates images based on variations in the phase of X-rays. This article describes using two types of instruments based on those different imaging methods to observe rubber during fatigue testing (Table 1).

Conclusion

Specimens for testing rubber fatigue were scanned using two types of X-ray imaging systems, a microfocus X-ray CT system and a phase-contrast X-ray CT system. By stretching samples, magnified images were acquired by the inspeXio SMX-225CT FPD HR Plus X-ray CT inspection system, and even small defects could be observed in detail and defect volume and count values compared at respective cycle count levels. The Xctal 5000 can determine the approximate orientation, size, and depth of microcracks without stretching samples or using magnified imaging. Both instruments can inspect items non-destructively, and the same specimen can be used to understand the progression of defects and cracks at any number of cycles. The characteristics of these instruments for scanning and analyzing data from specimens tested for rubber fatigue are indicated in Table 7.