News from LabRulezICPMS Library - Week 17, 2025

Our Library never stops expanding. What are the most recent contributions to LabRulezICPMS Library in the week of 21st April 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 Agilent Technologies and Shimadzu and other document by Thermo Fisher Scientific!

1. Agilent Technologies: Determination of Elements in a Solid Sulfide Electrolyte using ICP-OES

Analysis of next generation solid-state lithium-ion battery electrolyte chemicals by Agilent 5800 VDV ICP-OES

• Application note
• Full PDF for download

The rapid expansion of renewable energy sources and electric mobility usage is driving interest in the next generation of energy storage technologies. Currently, lithium-ion batteries (LIBs) are the leading storage method that is used across a wide range of applications. However, LIBs are limited by raw material availability and high costs, as well as concerns around safety. Solid-state batteries are emerging as an alternative energy storage technology. These batteries use a solid superionic material as the electrolyte instead of traditional liquid-phase electrolytes. This material, which transmits ions through a solid crystalline lattice, has the potential for high energy density compared to conventional batteries, as well as increased safety and operating temperatures.¹ Li10GeP2 S12 (LGPS) is one such inorganic solid electrolyte that is currently being investigated due to its high ionic conductivity. As with traditional battery electrolytes, the quality and purity of the solid electrolyte must be high to effectively facilitate ion transport. The presence of elemental contaminants could potentially affect the regular lattice structures of the electrolyte and impact battery longevity, lifespan, and safety.^2,3 

Spectroscopic techniques like Inductively Coupled Plasma-Optical Emission Spectroscopy (ICP-OES) are widely used to determine elemental contaminants in complex materials. The technique is especially useful for the simultaneous measurement of trace elements in samples such as battery electrolytes, due to its speed, sensitivity, and tolerance to high total dissolved solids (TDS). 

Both the Agilent 5800 Vertical Dual View (VDV) and 5900 Synchronous Vertical Dual View (SVDV) ICP-OES instruments have been adopted across the LIB value chain to address the varied analytical needs of the industry.4 Both instruments are ideal for labs dealing with novel materials, high numbers of samples, or aiming to make efficiency gains. In the absence of comparative methods for the analysis of LGPS, we focused on the development, optimization, and validation of the method to ensure the accuracy and reliability of the results. To support this process, we utilized the following hardware and software usability features to support the workflow throughout the study: 

• IntelliQuant Screening: The fast scan software feature was used to initially screen LGPS samples for elemental content across the entire wavelength range. The semiquantitative data provided valuable information on the identity of elements in the sample, enabled selection of appropriate analyte wavelengths, and helped establish suitable calibration ranges. 
• Early Maintenance Feedback (EMF): This software feature alerts the analyst when maintenance is required, based on a series of sensors, counters, and trackers. By maintaining optimum instrument operating conditions, unnecessary downtime is reduced, increasing the productivity of the instrument. 
• Intelligent Rinse: A feature that adjusts washout times based on the actual time it takes to wash out each element in the sample. This intelligent rinsing routine ensures that there are no carryover issues for problematic or high concentration elements. 

In this study, the 5800 VDV ICP-OES with an Agilent SPS 4 autosampler was used to determine 29 elements in battery grade LGPS electrolyte powder following microwave digestion. The elements included aluminum, arsenic, boron, barium, beryllium, calcium, cadmium, cobalt, chromium, copper, iron, gallium, germanium, potassium, lithium, magnesium, manganese, molybdenum, sodium, nickel, phosphorus, lead, sulfur, antimony, silicon, strontium, titanium, vanadium, and zinc.

Results and discussion

Calibration and linearity 

All 29 analytes were quantified using an external standard calibration method, with background correction performed by the instrument’s default and automatic Fitted Background Correction (FBC) routine. The FBC software corrects simple and complex background peaks automatically, requiring no input from the analyst. The results of the linear regression analysis of each analyte show excellent linearity across the calibration range with correlation coefficients ranging from 0.99900 to 1.00000 (Table 3). A representative spectrum and calibration curve for Cr 267.716 nm are shown in Figure 7.

Long-term stability 

To assess the stability of the 5800 VDV ICP-OES, 241 solutions were measured over eight hours without recalibration. The solutions consisted of 10 LGPS solutions and a QC block, which contained a rinse, Continuing Calibration Blank (CCB), and Continuing Calibration Verification (CCV) solutions. The CCV solution contained 0.250 mg/L of all analytes except Li, Ge, P and S, which were present at 250 mg/L. The recovery of the CCV was then plotted, as shown in Figure 8. The stability of all elements were within 100 ± 5%, with no QC failures over the entire analytical run. The precision of all elements, displayed as % Relative Standard Error (%RSD) was ≤2.5%, except As, which was ≤5%. The recovery data demonstrates the robustness of the 5800 VDV ICP-OES for the analysis of solid-state electrolyte material for over eight hours.

Conclusion 

The Agilent 5800 VDV ICP-OES with the Agilent SPS 4 autosampler was used to quantify 29 elements in 99.9% LGPS—a solid superionic material used as an electrolyte in solid-state LIBs. The samples were prepared using microwave digestion in reverse aqua regia and then analyzed by ICP-OES. With no previous methods available for reference, the following smart tools were used during the study to simplify method development and optimize the analytical workflow, ensuring consistent high-quality results throughout the analysis: 

• The IntelliQuant Screening method development tool was used to set an appropriate calibration range and to select the best wavelengths to use for the quantitative method. 
• Intelligent Rinse greatly reduced the analysis time by monitoring analyte intensities and rinsing for the minimum required time, while maintaining data accuracy. More than 60 minutes were saved for every 100 solutions using the intuitive rinse routine, compared to the standard 60-second rinse time per solution. 
• Early Maintenance Feedback alerted the analyst when maintenance was required based on real usage, maintaining optimum instrument performance and uptime.

The accuracy of the method was evaluated by conducting spike recovery tests of the LGPS sample. Recoveries were within 100 ± 10% in all cases, with precision (%RSD) of most elements below 2.5%. The instrument also displayed excellent stability over the eight-hour run without failing a single QC measurement. This study demonstrates that manufacturers of solid-state battery electrolytes can reliably and accurately measure impurity elements using the 5800 VDV ICP-OES.

2. Shimadzu: Multi-Element Analysis of Farmland Soil Extracts Using ICPE-9820 and a Multi-Component Extraction Method 

• Application note
• Full PDF for download

User Benefits:

• The ICPE-9820 can quickly analyze farmland soil for multiple elements simultaneously.
• The multi-component extraction method can be used for accurate analysis of even high salt samples (0.2 mol/L sodium chloride). 

Farmland soil contains constituents essential for crop growth, and their concentrations affect both yield and quality. Soil testing uses soil analysis to determine the concentrations of these constituents and the fertilization regimen needed to achieve an optimum balance of constituentsin farmland soil. 

Soil testing typically uses a different extraction process for each target analyte, requiring a large number of analytical operations, but a multi-component extraction method can be used to analyze multiple soil constituents with a single extraction process for quicker overall analysis. The Tokyo University of Agriculture soil testing system uses sodium chloride for multi-component extraction, enabling the measurement of exchangeable constituents (Al, Ca, K, Mg, P, and S) and inorganic nitrogen (ammonia nitrogen and nitrate nitrogen) and the estimation of cation exchange capacity (CEC) from the same solution extract. 

By measuring multiple elements simultaneously in a single analysis, The ICPE-9820, an inductively coupled plasma atomic emission spectrophotometer (ICP-AES) offers quicker elemental analysis. And it can be combined with sodium chloride extraction to dramatically reduces the time required to perform soil testing. 

In this Application News, the ICPE-9820 analyzed farmland soil solution extracts for exchangeable constituents, available boron and trace elements, and a spike recovery test and a dilution test were then performed to validate this analytical method.

Conclusion 

In this Application News, exchangeable components, available boron, and trace elements were analyzed in three farmland soil solutions extracted with extraction reagents used in the Soil Diagnostic System of Tokyo University of Agriculture using ICPE9820. The results from validation testing show the analytical method was accurate. And using an axial view and radial view of plasma for different purposes allowed high-concentration and low-concentration constituents to be measured simultaneously without diluting samples for individual target analytes.

3. Thermo Fisher Scientific: Pushing the limits for trace elemental analysis using triple quadrupole ICP-MS

• Other document (Case study)
• Full PDF for download

Ultra Trace Analysis Aquitaine (UT2A) was formed in 1999 as a spin-off laboratory from the University of Pau, France, and is today a renowned independent technology center dedicated to inorganic analysis. The team’s mission is to help their clients fully understand the elemental content of their samples—not just supporting them by performing analyses but also helping established laboratories develop and fully optimize existing methods, up to the generation of ready to implement SOPs. UT2A collaborates with customers from all industries and analyzes a wide range of samples, including waters, foods, pharmaceuticals, and polymers. UT2A also provides solutions to test established methods for evaluation of performance. 

Jean Dumont is an application engineer with a background in elemental speciation who is now managing the routine analysis performed in the laboratory. He joined UT2A in 2003 as one of the first of what is now a team of 11 technical experts and lab technicians in the field of elemental analysis. “The first ICP-MS I used did not yet have a collision cell, so we had to be very careful with interferences,” says Jean. He adds, “For us, it is also very important to include sample preparation into our considerations as it is vital to get complete digestions and also to decrease detetction limits due to backgrounds.” 

UT2A received a Thermo Scientific™ iCAP™ MTX ICP-MS in their lab and have used it intensively and in full production over a period of 10 months. This was possible as the system was fully qualified using IQ/OQ. The instrument was usually operated twice per week, and on each day of operation, approximately 200 samples were run, including all blanks, standards, and QC checks.