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Routine Analyses Through the Thermo Scientific ARL X'TRA Companion XRD

insights from industryRaphael Yerly, Simon WelzmillerXRD Product Manager & Application SpecialistThermo Fisher Scientific

In this interview, Raphael Yerly and Simon Welzmiller discuss how routine analyses can be powered by their Thermo Scientific ARL X'TRA companion XRD instrument.

What is the ARL X'TRA Companion X-ray diffractometer? Can you highlight a unique feature of ARL X'TRA Companion XRD that sets it apart from other instruments?

Raphael Yerly:

The ARL X'TRA Companion X-Ray Diffractometer is a powerful analytical instrument designed for X-Ray diffraction applications. One standout feature that sets the ARL X'TRA Companion apart is its unique 2D standard detector. This detector offers several advantages, including high count rates, excellent energy resolution, and the capability to achieve low background levels.

Using a 2D detector enables detailed snapshot pictures, providing insights into the quality of sample preparation. While 1D and 2D detectors show similar results for regular powder work, the Companion's 2D detector ensures superior statistics, making it the preferred choice for samples with small phases or quantities.

Can you explain some of ARL X'TRA Companion's safety features and why they are important during analysis?

Raphael Yerly:

Safety is a top priority in the design of the ARL X'TRA Companion, and the instrument incorporates several key features to ensure a secure analysis environment. One notable safety feature is related to regulatory changes that mandate no power to any electrical motors when the instrument door is open.

When the ARL X'TRA Companion's door is open, all motor power is automatically switched off, eliminating the risk associated with any mechanical movements. This design ensures the operator's safety, allowing them to place their hands within the instrument without concern for unexpected movements.

This safety measure is crucial, especially during sample handling and preparation, where operators may need to interact with the instrument. The ARL X'TRA Companion provides a secure analysis environment by complying with these regulatory changes and implementing safety features, reducing the risk of accidents and enhancing overall user safety.

In your opinion, what industries or applications can benefit the most from the ARL X'TRA Companion's capabilities?

Image credit: Thermo Fisher Scientific

Raphael Yerly:

In my opinion, the ARL X'TRA Companion's capabilities make it highly beneficial for various industries and applications. One notable sector is the cement industry, where the instrument addresses analytical challenges in cement analysis.

Cement and related materials are complex mineralogical mixtures, and the ARL X'TRA Companion excels in identifying and quantifying these components, even in the presence of peak overlap and amorphous phases. The instrument's versatility extends to mining applications, particularly for analyzing lithium salts from Salars.

It is valuable in assessing lithium carbonate's purity, a crucial raw material for lithium-ion batteries. Moreover, the ARL X'TRA Companion is adept at handling materials with large structural features, as showcased in applications involving fatty acids and mesoporous materials. Its performance in low-angle data analysis is particularly relevant for materials with significant structural characteristics.

The ARL X'TRA Companion's capabilities extend across industries, including cement, mining, and materials crucial for emerging technologies like batteries.

Could you explain the significance of low-angle data in X-Ray diffraction and share an example of a material where it is crucial?

Simon Welzmiller:

Low-angle data in X-Ray diffraction is essential for analyzing materials with large structural features. One significant example is the analysis of fatty acids, such as Silver behenate. These fatty acids form a 3D arrangement, and XRD can measure the distance between the chains of these fatty acids.

The resulting diffraction peaks appear at lower angles. In the case of Silver behenate, a peak at around 1.5 degrees 2 theta corresponds to the distance between the chains. This low-angle data provides valuable insights into the material's structure. Another example is mesoporous materials like SBA-15, consisting of a pattern of pores or cavities embedded in amorphous matrices.

In this case, the low-angle peaks arise from the pattern of pores, and precise low-angle data analysis is crucial for understanding the material's characteristics. Therefore, low-angle data analysis is powerful for investigating materials with large-scale structural features.

Can you elaborate on the analytical challenges in cement analysis and how the ARL X'TRA Companion addresses them, especially in terms of repeatability?

Simon Welzmiller:

Cement analysis poses several analytical challenges due to the complex mineralogical mixtures, with peaks overlapping from similar crystal structures and unit cells. Amorphous phases, especially in slags and decarbonized cement, add complexity. The ARL X'TRA Companion addresses these challenges effectively, providing exceptional repeatability and accuracy.

In the analysis of cement clinker, a NIST-referenced material, we performed 10-minute acquisitions with 21 repeats on the same sample. Despite the initial complexity shown in the overview scan, the ARL X'TRA Companion's high resolution and advanced algorithms allow for clear peak separation in the fingerprint region.

This enables the differentiation of polymorphs like M1 and M3 of C3S. The results, including repeatability values for various phases, demonstrate the Companion's ability to meet and exceed ASTM norms, ensuring reliable and precise cement analysis.

How does the calibrated peak list (CPL) method work in refining the amorphous content, particularly in the context of cement-clinker mixtures?

Simon Welzmiller:

The Calibrated Peak List (CPL) method is employed to refine the amorphous content in cement-clinker mixtures. This is a critical aspect, given the presence of amorphous phases that lack a crystalline structure.

This quantification method involves setting up a calibrated peak for the amorphous phase, typically derived from a sample with a known composition. This calibrated peak serves as a reference for similar samples.

We utilized the CPL method in cement-clinker mixtures on samples with varying slag content. For instance, with predefined mixtures of ordinary Portlandite Cement Clinker and slag, we created scans where the 50/50 mixture was a reference. The calibrated peak, discernible around 30 degrees, was utilized for further quantification.

The refined amorphous content obtained through the CPL method showed excellent agreement with the reference values from the mixtures. A slight deviation was observed as the slag content increased, but overall accuracy remained high. Integrated into the ARL X'TRA Companion, this method ensures robust refinement and accurate determination of amorphous content in complex mixtures, such as those found in cement analysis.

Moving into the mining industry, can you discuss the specific challenges and solutions for analyzing lithium carbonate from Salars using the ARL X'TRA Companion?

Simon Welzmiller:

Analyzing lithium carbonate from Salars presents unique challenges due to the diverse processes involved in its generation. Lithium carbonate, a critical raw material for lithium-ion batteries, can be derived from either heavy rock mining (hard rock mining on Spodumene ore) or Salars, salt lakes where lithium-rich brine is processed.

There are two distinct samples to consider in the case of lithium carbonate from Salars. The first sample is a relatively pure lithium carbonate, where no crystalline phase is detectable via X-Ray diffraction (XRD).

The lithium content in this sample was found to be 18.8 weight percent, closely aligned with the value of 18.5 weight percent derived from elemental analysis. The agreement between the XRD results and elemental analysis indicates the effectiveness of the Companion in accurately determining lithium content.

The second sample, however, contains additional crystalline phases, including chlorides and sulfates. Despite the added complexity, the ARL X'TRA Companion facilitated a quantitative phase analysis through its robust XRD capabilities.

The lithium content in this sample was determined to be 18.0%, with a reference value from elemental analysis being 17.2%. The major elements, such as chlorine and sodium, were also detected, showcasing the ARL X'TRA Companion's versatility in handling mining-oriented materials like lithium carbonate from Salars.

The advantages of the ARL X'TRA Companion lie in its quick and straightforward analysis, requiring minimal sample preparation, and the ability to provide accurate results even in the presence of additional crystalline phases, demonstrating its efficacy in the mining industry.

Direct Reduced Iron (DRI) plays a crucial role in steelmaking. How does the ARL X'TRA Companion contribute to analyzing different phases in DRI, especially considering oxidation states?

Simon Welzmiller:

Direct Reduced Iron (DRI) is a pivotal intermediate product in the steelmaking industry, and its analysis is essential for process control, particularly regarding the metalization ratio, which represents the proportion of metallic to total iron. The ARL X'TRA Companion provides detailed insights into the different phases present in DRI, considering various oxidation states.

We analyzed two distinct samples of DRI, one with high metalization (97.7%) and another from an earlier process stage with lower metalization (93.7%). The analysis revealed the metallic iron content and the presence of iron oxides, such as hematite, magnetite, and Wuestite, each displaying different oxidation states of iron.

What sets the ARL X'TRA Companion apart is its ability to detect subtle variations in the phases. For instance, a more profound phase analysis identified a variant of Wuestite with less iron in a specific peak, indicating incomplete reduction from magnetite to Wuestite. By incorporating this information into the refinement process, the ARL X'TRA Companion achieves a more precise quantification, resulting in adjustments to the content of different phases.

This level of detailed analysis is crucial for obtaining accurate results in quantifying various phases in DRI, reflecting the ARL X'TRA Companion's capability to contribute significantly to process control in the steelmaking industry.

How flexible is the ARL X'TRA Companion in terms of acquisition time, and what factors influence the decision on the duration?

Simon Welzmiller:

The flexibility of the ARL X'TRA Companion in terms of acquisition time is a notable feature, allowing users to adapt based on specific analytical requirements.

For a cement clinker analysis, we conducted a 10-minute acquisition, emphasizing the high repeatability achieved within this timeframe. A cement sample analysis was demonstrated with a five-minute reduced acquisition time, still yielding satisfactory results. The key consideration here is the trade-off between analysis time and the desired level of statistical confidence.

Factors influencing the decision on acquisition time include the sample type, the phases of interest, and the required precision. In cases where shorter analysis times are acceptable, the ARL X'TRA Companion proves adaptable without compromising the reliability of results. However, it is essential to assess the specific requirements of the analysis and strike a balance between the time invested and the desired level of accuracy and repeatability.

How does one ensure accuracy when working with samples that lack certified values for comparison?

Raphael Yerly:

Ensuring accuracy in the absence of certified values for comparison can be challenging. Accuracy is typically determined by comparing measured values to certified ones. However, if certified material is unavailable, it becomes difficult to provide a precise accuracy statement.

One can optimize the analytical method using known materials, like NIST Clinkers, to validate and fine-tune the approach. By testing the method against materials with known values, you can gain confidence in the accuracy of the results. It is important to note that the accuracy can vary based on factors such as the type of phases, sample preparation, and the specific application.

Could you explain why sample freshness is crucial, especially for free lime measurements?

Raphael Yerly:

The freshness of the sample significantly influences the accuracy of free lime measurements. Free lime is a phase that can change over time due to aging. When working with certified materials like NIST Clinkers, which may have been manufactured years ago, the free lime content may deviate from the certified values.

For precise and reliable free lime measurements, it is essential to use fresh samples that have not undergone significant changes or aging. This ensures that the free lime content in the sample represents its actual state, providing more accurate results during the analysis.

Can you explain the specialized sample holder for clays and how the ARL X'TRA Companion ensures accurate measurements for clay phases?

Raphael Yerly:

Clays indeed have unique characteristics, and the ARL X'TRA Companion is equipped to handle their analysis effectively. One of the considerations for accurate clay analysis is the specialized sample holder designed for this purpose.

The specialized sample holder for clays is tailored to accommodate the specific nature of clay samples, ensuring proper sample alignment and stability during analysis. This holder is optimized to enhance the accuracy of measurements, particularly for clays that may have distinct structural features.

The ARL X'TRA Companion's geometry and capabilities, combined with the specialized sample holder, allow for precise measurements of clay phases. The instrument's ability to start at very low angles further facilitates the analysis of clay materials, ensuring that even materials with large structural features can be accurately characterized.

Are there any upcoming developments or enhancements planned for the ARL X'TRA Companion that users should be excited about?

Simon Welzmiller:

Thermo Fisher is continuously working on enhancing our instruments, including the ARL X'TRA Companion X-Ray diffractometer. Our commitment to innovation means that users can look forward to future updates and improvements that will further enhance the capabilities and performance of the ARL X'TRA Companion.

We encourage users to stay informed about announcements or product updates through our official channels. We are dedicated to providing cutting-edge solutions, and users can anticipate exciting developments that align with the evolving needs of the analytical community.

How can customers reach out for support or further information regarding the ARL X'TRA Companion, and what support channels are available?

Raphael Yerly:

Customers can easily reach out for support or additional information regarding the ARL X'TRA Companion through various channels. They can contact their official demo representative in their territory, reach out directly to the factory, or visit our website for more details.

We are committed to providing comprehensive support, and our team is readily available to address any inquiries, offer guidance, or provide further information about the ARL X'TRA Companion X-Ray diffractometer. Whether through local representatives or direct communication with the factory, we aim to assist our customers effectively and ensure a positive experience with our instrument.

Watch the full webinar

About the interviewees: 

Raphael Yerly is a seasoned professional in the field of XRD (X-ray diffraction) instrumentation, with over 23 years of experience at Thermo Fisher Scientific, the world leader in serving science. 

Holding a degree in engineering from the Swiss Federal Institute of Technology, Raphael Yerly combines technical expertise with business acumen, having also earned an MBA. Recognizing the importance of using finite resources efficiently, Raphael has been actively involved in developing innovative solutions that enhance productivity and sustainability, particularly for industries such as cement, minerals, and metals.

Simon Welzmiller is a Global Application Specialist for X-ray diffraction at Thermo Fisher Scientific since 2017. He has more than 10-year experience in various XRD applications and techniques. 

Simon holds a PhD in Solid State Chemistry from Leipzig University and a master’s degree in chemistry from LMU Munich. After his Ph.D. thesis, he started a position as an Application Specialist for XRD with STOE. In 2017, he joined Thermo Fisher as an Application specialist for XRD. 

This information has been sourced, reviewed and adapted from materials provided by Thermo Fisher Scientific - Elemental Analyzers and Phase Analyzers.

For more information on this source, please visit Thermo Fisher Scientific - Elemental Analyzers and Phase Analyzers.

Disclaimer: The views expressed here are those of the interviewee and do not necessarily represent the views of AZoM.com Limited (T/A) AZoNetwork, the owner and operator of this website. This disclaimer forms part of the Terms and Conditions of use of this website.

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