News from LabRulezICPMS Library - Week 38, 2024

Our Library never stops expanding. What are the most recent contributions to LabRulezICPMS Library in week 39, 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, Thermo Fisher Scientific, and Metrohm!

1. Thermo Fisher Scientific: Analysis of process water from hydrogen fuel cells using triple quadrupole inductively coupled plasma mass spectrometry (ICP-MS)

• Application

Goal

To demonstrate the analysis of process water from hydrogen fuel cells for inorganic trace contaminants with high sensitivity and accuracy using triple quadrupole ICP-MS.

Introduction

The reduction of CO₂ emissions is a major task for societies globally as the rise of CO₂ in the atmosphere plays an enormous role in global warming. The automotive industry mainly focuses on the transition from petrol-fueled to electric vehicles (EVs) to reduce emissions; however, the generation of energy and energy-intensive industrial processes are also important sources of emissions. Here, other ways of reducing CO₂ emissions might be feasible, and in the center of current debate stands the use of (ideally green) hydrogen and its combustion in hydrogen fuel cells. Hydrogen fuel cells are one of the key technological developments as there is no emission other than water. In addition, hydrogen can be created using renewable energies and can be transported with low effort due to its low density of only 70.85 g·L^-1 when liquified.

A typical hydrogen fuel cell consists of two electrodes (anode and cathode) and a polymeric electrolyte membrane (PEM) as shown in Figure 1. Typically, the electrode is made from fluorinated polymers to allow for chemical and mechanical stability and coated with a catalyst. Platinum is the catalyst material offering the highest efficiency; however, it is expensive. To reduce the production cost, improving the platinum coating technology and monitoring potential degradation by means of metal release into the water produced in the process are important. Due to the use of material blends, different trace metals as well as other non-metal contaminants must be monitored.

In general, inductively coupled plasma mass spectrometry (ICP-MS) is the preferred analytical technique for the analysis of metals and related contaminants down to sub ng·L^-1 levels. However, non-metals such as phosphorous or sulfur are challenging to analyze using ICP-MS due to a combination of their usually elevated ionization potentials and significant spectral interferences. Current hydrogen fuel cell technology uses mineral acids, like sulfuric acid, as electrolytes with a platinum catalyst on the electrodes (PAFC). Thus, it is important to monitor the concentrations of these elements at low concentrations. Oxygen- and nitrogen-based polyatomic interferences are usually of greatest concern for these analytes, but other polyatomic interference, like ³¹P¹H⁺, may lead to false positive results and must be removed.

Another challenge is the analysis of fluorine, which is also a key analyte for monitoring degradation of the PEM. Fluorine has the third highest first ionization potential of any element in the periodic table (behind neon and helium). In addition, its only naturally occurring isotope, ¹⁹F, falls into a severely interfered mass range, mainly due to the interferences generated by naturally abundant ions such as H₃O⁺ and peak tailing of H₂O⁺. To overcome these challenges, fluorine can be measured indirectly after mixing the sample with a solution containing barium. This results in the formation of ¹³⁸Ba¹⁹F⁺ in the plasma, allowing the fluorine concentration to be measured interference free via m/z 157. Because of the required setup, the analysis of fluorine has to be conducted in a separate measurement and cannot be combined with the analysis of the other contaminants.

In this study, a Thermo Scientific™ iCAP™ TQe ICP-MS was used for the analysis. Use of triple quadrupole technology offered superior interference removal and facilitated the analysis of important contaminants, including fluorine, at ultra-trace levels in the water produced by hydrogen fuel cells

2. Metrohm: Optimize raw material identification and verification (RMID) with MIRA P

• Application

Validation model transfer increases productivity

Using a verification model on multiple instruments expands a manufacturer’s raw material identification/ verification (RMID) capabilities by speeding up incoming inspection, imparting flexibility to an operation, or avoiding downtime.

In a scenario where several operators use multiple MIRA P systems at different locations, the ability of any operator to use any MIRA P to validate a new shipment streamlines operations and allows that shipment to be quickly released to production. In most cases, a well-designed model with inherent sample variability can be built on one MIRA P and transferred to another. In some cases, variance must be added to a training set with a few additional samples. This Application Note describes how a model transfers from one MIRA P to another in order to scale MIRA P usage across an entire operation.

INTRODUCTION

Model building (including training and validation set samples, operating procedure (OP) settings, and necessary variance) has already been well-established for RMID with a unique MIRA P [1,2].

In summary, MIRA Cal P generates PCA-based (principal component analysis) models using Training Set data and Operating Set parameters to verify target substances. Ideally, a model can be created on one instrument («MIRA P 1»), downloaded onto a second instrument («MIRA P 2»), then validated on the second unit and used directly.

The model must be expanded if the initial transfer does not produce satisfactory p-values or does not pass validation. This involves introducing variance in the model and/or optimizing model parameters and/or ensuring consistent usage by each operator of the instrument.

CONCLUSION

The benefits of using multiple MIRA P devices for raw material verification include smoother operations and faster turnaround of products. This Application Note is intended to guide users through model transfer and enable the deployment of multiple MIRA P instruments. From tips for the simplest transfer to tools for more challenging tasks, we want you to be confident in taking your inspection with MIRA P to the next level. This flowchart is a quick reference for the basic flow of operations during MIRA P to MIRA P transfer.

3. Agilent Technologies: Fentanyl Detection Using an Agilent Resolve Handheld Raman Analyzer

• Application

Safe identification of novel illicit opioids

Fentanyl and fentanyl analogs are highly potent synthetic opioids that were developed in the 1950s as analgesics. These drugs are approved for clinical and veterinary use due to their rapid onset, potency (10 to 10,000 fold higher potency than morphine), and variety of administration methods.¹ However, these highly potent substances are increasingly found on the illicit drug market in North America², where they have contributed significantly to the "opioid crisis" and to a high number of overdose-related deaths. Illicit fentanyls are available as powders, tablets, liquids, or skin patches, and have been found with other psychoactive substances, including heroin, cocaine, and methamphetamine.³ All these material types present a high risk both in their pure form and after they have been prepared and packaged for sale.

The Agilent Resolve handheld Raman analyzer uses spatially offset Raman spectroscopy (SORS) technology to identify hazardous materials, explosives, and narcotics concealed behind single and multiple barriers. These barriers can include colored and opaque plastics, glass, paper, cardboard, wrapping, and fabrics. The combination of SORS, high data quality, low fluorescence interference, and a spectral library that is continuously updated with new psychoactive substances makes the Resolve a powerful tool in the detection and identification of controlled substances. As of library version 41, over 70 different fentanyls can be identified using Resolve.

4. Shimadzu: Evaluation of TOC of Sulfuric Acid using Wet Oxidation TOC Analyzer

• Application

User Benefits

• It is feasible to quantify low TOC content in 10 % sulfuric acid solution and thereby manage organic contamination within sulfuric acid solutions.
• By using the auto-sampler, multiple samples can be automatically measured.

Introduction

Sulfuric acid is one of the chemicals used in the semiconductor industry for precision cleaning of surfaces such as wafers. When the cleaning solution is contaminated with organic impurities, it may not only affect the objects being cleaned but also the manufacturing process itself. Therefore, stringent quality control is imperative for the sulfuric acid utilized in the cleaning process.

Organic impurities in sulfuric acid can be evaluated by measuring total organic carbon (TOC). The wet oxidation TOC analyzer, which is capable of high-sensitivity TOC measurement, is effective for managing trace organic substances required by the increasing complexity of integrated circuits. This article introduces an example of TOC measurement conducted with the Shimadzu wet oxidation total organic carbon analyzer TOC-V on a 10 % sulfuric acid solution.

Conclusion

The capability to measure low-concentration TOC in 10 % sulfuric acid solution by using the wet oxidation total organic carbon analyzer TOC-V is confirmed. When high-purity sulfuric acid is required, as in industries like semiconductor manufacturing, the use of the wet oxidation TOC-V analyzer can facilitate the management of organic impurities in sulfuric acid, offering the potential for its utilization in quality assessment. Additionally, the use of an autosampler enables the automated measurement of multiple samples, contributing to improved analytical efficiency.

Furthermore, application news 01-00535 introduces the combustion catalytic oxidation TOC-L analyzer, which is used to measure TOC in approximately 1 % sulfuric acid solution.