News from LabRulezICPMS Library - Week 8, 2025

Our Library never stops expanding. What are the most recent contributions to LabRulezICPMS Library in the week of 17th February 2025? Check out new documents from the field of spectroscopy/spectrometry and related techniques!

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

1. Agilent Technologies: ICP-OES Quality Control of Elements in Brines Produced by Direct Lithium Extraction (DLE)

Automated analysis of lithium brines using an Agilent ICP-OES Automation System

• Application note
• Full PDF for download

Direct Lithium Extraction (DLE) technology is a selective process designed to recover lithium (Li) from underground raw Li brine deposits while removing impurities.¹ Compared to conventional Li extraction methods, such as mining hard rock ores or using brine evaporative methods, DLE is faster, consumes less water and power, produces less waste, and requires less land. Given these process and sustainability advantages, DLE is gaining significant attention from industry, academia, investors, and environmentalists.

Agilent ICP-OES Automation System

Robust instrumentation is therefore needed for the routine elemental analysis of large numbers of brine samples. An Agilent ICP-OES Automation System comprising the Agilent 5900 SVDV ICP-OES, Advanced Valve System (AVS 7), Advanced Dilution System (ADS 2), SPS 4 autosampler, and instrument software was used in this study. The Agilent 5800 VDV ICP-OES is also suitable for this application. 

The 5900 ICP-OES uses a vertical plasma torch and a solid-state radio frequency (SSRF) generator operating at 27 MHz to create a plasma with the stability needed for the routine analysis of brines. The integrated AVS 7 switching valve ensures fast analysis times and reduces instrument exposure to solids in high TDS samples.³ The accessory also minimizes carryover from sodium (Na) and prevents excessive torch devitrification, greatly reducing the frequency of instrument cleaning and extending the lifespan of parts.

The samples analyzed in this study were produced using a membrane-based DLE methodology and included a wide variety of sample matrices, with target analytes typically present across a broad range of concentrations. Some key analytes, such as Li, Na, and magnesium (Mg), are particularly important to quantify as they directly impact the efficiency of the DLE process. 

To account for the different compositions and densities of the DLE samples, the ADS 2 was used to prepare calibration standards across a wide analytical range and to dilute the samples before analysis.⁴ Both processes can be labor-intensive and time-consuming when performed by an analyst, as well as being potential sources of contamination and errors. The implementation of advanced autodilution technology for ICP-OES enhances sample turnaround time and minimizes the risk of human errors, while ensuring accurate results.

Conclusion

An Agilent ICP-OES Automation System comprising the Agilent 5900 SVDV ICP-OES, AVS 7, ADS 2, SPS 4 autosampler, and ICP Expert Pro instrument software was used to analyze 12 elements in real brine samples. The raw, tail (Li-free), and Li concentrate brine samples were sourced from before and after processing using a membrane-based Direct Lithium Extraction (DLE) technique. All samples were analyzed using a single method in a single run.

The IntelliQuant Screening method development tool within the software was used to set the calibration range for the analytes and to select the best analyte wavelengths. The use of the ICP-OES Automation System provided productivity and performance benefits for the brine application including:

• Automatic calibration. Completely automated calibration from three stock solutions removed the need to manually prepare standards to cover the wide and varying concentration range of analytes in the brines.
• Prescriptive dilution. The ADS 2 was used to automatically dilute all three of the Li brine samples 50 times, so that the samples could be measured in a single run.
• Reactive dilution. The ADS 2 automatically diluted the Li concentrate brine sample 200x in response to the concentration of Li exceeding the calibration range before remeasurement.
• The ADS 2 also performed reactive dilutions on the raw brine (150x) and the tail brine (250x) to quantify Na.
• Results summary report. The software selected the best measurement results to display from the available reactive dilution remeasurement results. It allowed for straightforward data viewing and reduced the amount of time required for manual data processing.
• The AVS 7 minimized the exposure of the torch, nebulizer, and pump tubes to the high matrix samples. It also worked seamlessly with the ADS 2 to improve sample turnaround times.

2. Bruker: IR-Spectroscopic Analysis of Polymer Fillers and Compatibilizers

• Application note
• Full PDF for download

Many of today’s plastics are multi component systems with multiple constituents like different polymers, fillers, plasticizers and compatibilizers. By systematic selection and blending of these constituents in appropriate mixture ratios tailor made substances with optimized material properties can be made. An important topic for quality control and analytical purposes is the identification and quantification of the individual components present in such plastics. 

Fourier transform infrared (FT-IR) spectroscopy is one of the fastest and most accurate methods for the analysis and quality control of polymers. High quality IR spectra can be recorded in a few seconds; usually there is no need for sample preparation or costs for expensive consumables. Within only a minute FT-IR spectroscopy allows to verify that a given product is within its specification or to quantify one or more of its constituents.

Measurement approach

Nowadays, quality control and routine analysis using IR spectroscopy is mainly performed applying the ATR (Attenuated Total Reflection) technique. As there is virtually no sample preparation required ATR is much more comfortable to use than the conventional transmission mode. For the analysis the sample has to be pressed on the ATR-crystal, which is the measurement interface. From the ATR-crystal, the IR radiation penetrates slightly (a few microns) into the sample surface. The IR detector of the FT-IR spectrometer can then measure the absorbance resulting from the sample. The ATR-technique can be applied for almost all types of samples (e.g. solids, liquids, powders, pastes, pellets, slurries, fibres etc.). The analysis takes less than a minute, including sampling, measurement and data evaluation. By using ATR, it is even possible to differentiate between the top layers of a polymer laminate, which cannot be achieved in transmission mode.

Instrumentation

The very compact ALPHA II FT-IR spectrometer with the high pressure Platinum diamond ATR-module is a robust and affordable system that is very easy to operate. Diamond is a very hard-wearing, chemically inert and therefore ideal material for the analysis of a wide range of samples. In the platinum ATR-module the diamond is brazed into tungsten carbide. This extremely robust design allows the application of very high pressure so that even the hardest plastics can be measured. For the measurement of highly absorbing dark samples (e.g. black polymers) and thin layers an ATR-material with a high refractive index is required to limit the penetration depth of the IR-light into the sample. Therefore the Platinum ATR module can be equipped with a germanium (nGe = 4.0) crystal plate. To provide the user an unobstructed access to the sampling area, the pressure applicator can be rotated by 360°. The software is very intuitive and a software wizard guides the user through the analysis procedure.

Summary

The combination of Bruker Optics compact and robust FT-IR spectrometer ALPHA II with a high pressure diamond ATR unit is an ideal tool to analyze polymers, fillers and polymeradditives. The system allows quantifying single components in complex mixtures. The setup of new methods even for chemically similar polymers is quick and straightforward. A very intuitive work flow allows even spectroscopically inexperienced users to perform the analysis.
Altogether the ALPHA II is perfectly suited for the identification of fillers, the quantification of mixture components and the quality control of polymers.

3. Metrohm: Moisture content and rheology determination of fluorinated polyolefins using NIRS

Moisture and melt flow rate analysis results within seconds

• Application note
• Full PDF for download

Ethylene tetrafluoroethylene (ETFE) is a partially fluorinated copolymer of ethylene and tetrafluoroethylene. ETFE is a melt processable polymer, designed to have high corrosion resistance and strength over a wide temperature range. Some key quality parameters that should be monitored during the production of fluorinated polyolefins are melt flow rate (MFR) and moisture content. The measurement of these parameters usually involves using chemicals and can be time-consuming. Nearinfrared spectroscopy (NIRS) offers users rapid and reliable prediction of key quality parameters in ETFE without any sample preparation or cleaning procedures. 

Experimental equipment

273 ETFE pellet samples with varying MFR and moisture content were measured on a Metrohm nearinfrared spectroscopic analyzer in reflection mode. All measurements were performed in rotation using a large sample cup to reduce the stray light effect caused by varying particle sizes. An overlay of the sample spectra is displayed in Figure 1.

Conclusion

This Application Note demonstrates the feasibility to determine mechanical properties and perform moisture analysis in fluorinated polyolefins like ETFE using NIRS. In comparison to the standard analytical methods (Table 1), quality control with NIR spectroscopy shows obvious advantages regarding the analysis time. In addition, the sample handling with near-infrared spectroscopy is easier to perform and safer since no chemicals are needed.

4. Shimadzu: Quantitative Analysis of Copper Alloys and Differentiation of Sample Types by Matching Function

• Application note
• Full PDF for download

User Benefits

• The EDXRF has a smaller footprint than the WDXRF, and does not require cooling water or other auxiliary equipment.
• Analyses can be carried out simply without tedious and time-consuming sample preparation because there are few limitations on the sample shape.
• Sample types can be differentiated by using the matching search function provided as a standard feature

Copper alloys are copper-based alloys which are produced by adding zinc, lead, tin, or other alloying elements to copper to improve machinability, wear resistance, corrosion resistance, or other properties. By composition, copper alloys are classified as the 1000 seriesto the 7000 series. Energy dispersive X-ray fluorescence spectrometers (EDXRF) are widely used in applications such as receiving inspections of recycled materials, taking advantage of their excellent operability and simple sample handling, but high-accuracy wavelength dispersive X-ray fluorescence spectrometers (WDXRF) are used mainly in metal manufacturing processes. However, as a result of improvement in the quantitative accuracy of EDXRF in recent years, a wider range of applications, such as use in manufacturing processes, is expected in the future. This article introduces an evaluation of the analytical performance of the Shimadzu EDX-7200 in an analysis of copper alloys, focusing on the following items.

• Quantitative analysis by the calibration curve method (accuracy of calibration curves, lower limit of quantitation, repeatability)
• FP (fundamental parameter) qualitative/quantitative analysis and matching function

Conclusion

This article has introduced an evaluation of the analytical performance of the EDX-7200, using copper alloys as an example. In the quantitative analysis by the calibration curve method, repeatability was evaluated, showing that results with high reliability can be obtained. The qualitative/quantitative analysis by the FP method also showed that samples can be differentiated easily by using the matching search function of the EDX-7200. Thus, the EDX-7200 offers a combination of merits. In addition to excellent analytical performance and a small installation footprint, there is no need cooling water or other auxiliary equipment, there are few limitations on the sample shape, and highly accurate analysis of samples even in their original shape is possible. Based on these advantages, It is expected that EDX-7200 will be widely used to replace analysis using WDXRF.

5. Thermo Fisher Scientific: Reliable and productive analysis of food samples using single quadrupole ICP-MS 

• Application note
• Full PDF for download

Inductively coupled plasma mass spectrometry (ICP-MS) is the technique of choice for accurately measuring toxic elements, especially for analytical testing laboratories. At the same time, it also allows the analysis of major nutritional elements present in concentrations several orders of magnitude higher. However, sample matrix variability and the large sample load usually found in testing laboratories may lead to challenges like unstable internal standard recoveries outside acceptable ranges, quality control failures and drift, rapid degradation of instrument performance. If left unaddressed, these may cause unexpected downtime and interruptions to the overall laboratory productivity.

This study describes how the Thermo Scientific™ iCAP™ MSX ICP-MS instrument, equipped with argon gas dilution (AGD), is able to reliably overcome these challenges and enables seamless multielement analysis of different kinds of food samples with simplicity.

Conclusion

This study demonstrates how the iCAP MSX ICP-MS fulfils the requirements of food testing laboratories and resolves the typical challenges associated with this sample type. Close to 7,000 food samples were measured in this study over eight weeks where daily sequences ran for more than 12 hours with stable data, negligible analytical drift, excellent internal standard response, and without the need for any maintenance actions.

• The use of AGD allowed effective handling of matrix and compositional variability introduced by widely different food samples, commonly analyzed together on the same day in analytical testing laboratories.
• Accuracy and precision were demonstrated using applicable certified reference materials, which were successfully analyzed and quantified with excellent recoveries.
• High concentrations of nutritional elements were accurately measured alongside accurate quantification of low-level toxic elements in the same samples.
• Specially challenging elements like arsenic, typically expected in the range of a few µg·kg-1 or lower in food samples were measured and quantified using He-KED mode. Mathematical correction using half mass signals was further used to reduce the impact of rare earth elements, potentially present in some samples.