News from LabRulezICPMS Library - Week 15, 2025

Our Library never stops expanding. What are the most recent contributions to LabRulezICPMS Library in the week of 7th 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, Bruker Optics and Shimadzu and brochure by Anton Paar!

1. Agilent Technologies: Supporting Continuous Manufacturing of Drug Products with Transmission Raman Spectroscopy

Fast at-line analysis using an Agilent TRS100 adds analytical insight to existing in-line PAT

• Application note
• Full PDF for download

In this work, Agilent collaborated with the tablet press and CM equipment manufacturer Fette (Schwarzenbek, Germany)8 , in a joint demonstration of the capabilities of our respective at-line and in-line testing technologies. 

The Fette continuous processing system (FE CPS) and tablet press (FE55) is a complete continuous direct compression (CDC) system. It applies fully-integrated in-line NIR blend uniformity (BU) of the powder and Tablet Uniformity (TU) sensors on the individual tablets that are pressed from the equipment. The CPS system features advanced in-line NIR process analysis technology (PAT), enabling continuous monitoring and direct adjustment of the production process. 

Based on the guidance described in ICH Q13, a fast, at-line, bulk reference testing technique is also needed to validate and verify the PAT's performance and to verify that TU is equivalent to CU. To complement the in-line NIR PAT, the TRS100 was evaluated for CDC deployment, process optimization, process validation, and ongoing verification of the commercial process. 

The objective of this study was to use the TRS100 to analyze tablet core samples produced by the FE55 and to compare the data to results obtained by the Fette in-line PAT (ePAT) and offline HPLC.

Results and discussion

Applying the quick and fine-tuned calibration methods to CM samples 

To assess the consistency in the CM process and the predictive performance of the analytical methods, the two calibration models were used to predict the API % w/w value of the remaining 262 CM samples. The narrow range and low RSDs of the results presented in Figure 8 and Table 3 show the highly consistent predictive performance of both TRS methods. The results confirm the suitability of the technique for at-line testing of OSD forms and for verifying the performance of the in-line NIR PAT.

Comparison of TRS and PAT data 

A final comparison of the TRS data from the fine-tuned model with the Fette inline TU sensor of the CDC system, measuring every single tablet produced during the 24-hour continuous run, is shown in Figure 9. The results show that the performance of the TRS closely aligns with that of the Fette NIR TU sensor in a consistent manner with low variation. Greater variation in the data acquired using the Fette NIR ePAT sensors is expected due to faster acquisition times of 3.8 ms for each tablet, resulting in 4,197,271 concentration points (Figure 9). The tighter clustering of the TRS data is expected due to the longer, 10-second, acquisition times and transmission measurements through the sample volume reducing sub-sampling.

Conclusion

This study demonstrates the effectiveness of the Agilent TRS100 as an at-line analytical technique for bulk predictive sampling of oral solid dose forms, supporting continuous direct compression (CDC) in pharmaceutical manufacturing. 

The quantitative data produced by the TRS100 also confirmed the performance of the Fette inline process analysis technology (ePAT) system. Using an at-line method to validate and verify the PAT system is faster and more cost-effective than traditional offline wet chemistry techniques, which are performed in a separate QC laboratory. 

The TRS100 showed that tablet uniformity (TU)—obtained through inline diffuse reflectance NIR of the PAT—is equivalent to content uniformity (CU), as determined using offline transmission Raman spectroscopy. 

TRS adds value by supporting the CDC process development and enhancing process understanding, even with rapid calibration methods developed in less than three hours. It also demonstrates consistent results on the whole sample, compared to inline measurements that only analyze a subsample of a tablet.

2. Anton Paar: Solutions for Ore Refining and Processing (Mining Industry)

• Brochure
• Full PDF for download

Responsible and Sustainable Production for High-Quality Products

Sustainable mining of natural resources is a cornerstone of our standard of living and prosperity. With a wide range of applications, mined materials play a critical role in various segments of our lives, including construction and power generation, and are used as commodities for industrial applications and luxury goods. They also contribute to current green technologies – like wind turbines, solar panels, and electric vehicles – and are an integral aspect of the effort to counter climate change. Exploring new exploitable deposits and recycling raw materials have to be done responsibly for mining to have a sustainable economic role in society. Mined metals and minerals must be extracted, transported, stored, and processed according to quality control processes that deliver safe and high-quality products. We have a wide array of instruments that contribute to every step of this development and production chain.

Anton Paar Instruments 

XRDynamic 500 

XRDynamic 500 ensures optimized processes at every stage of the mining operation via rapid as well as precise phase identification and quantification of metals and minerals. 

• Right out of the box: Best-in-class resolution / signalto-noise ratio 
• TruBeam™ concept: Larger goniometer radius and evacuated beam path 
• Full automation: X-ray optics and beam geometry change

Ultrapyc series 

Measurements with the Ultrapyc gas pycnometers take less than 10 minutes, so they’re perfect for controlling the quality of your solid materials and slurries throughout exploration and processing. 

• PowderProtect: Measure fine powders without instrument contamination 
• Built-in Peltier temperature control for superior thermal stability 
• Accurate results for sample volumes from 4.5 cm3 to 135 cm3

Multiwave GO Plus, Multiwave 5000, Multiwave 7101/7301/7501 

Multiwave digestion systems are the perfect sample preparation instrument for the mining industry. 

• Budget-friendly disposable vials and inserts for economic sample preparation 
• Innovative features (e.g., library with more than 500 methods, hands-free door opener) make microwave digestion easier and more convenient than ever 
• Clever instruments and vessel concepts, state-ofthe-art sensor technology, and the highest safety standards (ETL and GS safety certificates)

PSA series 

The PSA instrument has market-leading robustness when it comes to ground vibrations, dusty environments, and abrasive samples. 

• Permanently aligned solid-state lasers – durable and resistant to ground vibrations 
• No glass in the dry path of the sample and exceptionally robust glass in the liquid path 
• Compact 2-in-1 design to conduct both wet and dry measurements in a single setup

MCR rheometer series

Your solution for material flow optimization, from designing raw material powder transport to predicting flow behavior of tailings suspensions and optimizing slag processing. 

• 15 rheometers and over 200 accessories mean all of your samples and requirements are covered 
• A range of smart features do the work so you can do the thinking 
• Continuous development of the portfolio in response to customer feedback and new ideas

ViscoQC, RheolabQC 

For quick and convenient dynamic viscosity measurements, ViscoQC and RheolabQC rotational viscometers ensure the quality of your substance for the best pumpability and workability results. 

• Save time with the fast and highly accurate sample temperature control delivered by the Peltier temperature devices PTD 80 and PTD 175 
• Unique features provide error-free and efficient operation 
• Economical consumption of resources with a small footprint

3. Bruker Optics: FT-NIR-Spectroscopy for Process Monitoring of Polymers

• Application note
• Full PDF for download

FT-NIR spectroscopy has a distinct advantage compared to other technologies: It provides a real-time assessment of the process on a molecular basis. The recorded spectra relate directly to the composition of the material. With the use of fiber-coupled probe heads, the “eye” is brought straight into the area of interest without interference in the production process. The spectrometer itself can either be installed alongside the measurement point or further away in the analysis house. 

Modern control software hands the data over to the process control system and if the product is running out of specification, it will be detected within seconds and corrective measures can be carried out. With the classical off-line analysis, several hours can pass before the sample is analysed. During that time the production of material with unknown quality continues; the longer the analysis time, the more waste could be produced. 

Recent advances in the development of new high temperature and high pressure probes allow the adaptation into various processes. The classical transmission probes of stainless steel or Hastalloy with sapphire windows are suitable for most translucent liquid systems. When the system is more scattering or opaque, like polymer melts, powders or pellets, diffuse reflection probes are favored. With direct insight into the molecular structure of the material, parameters like OH-number, NCO-content, Acidvalue, or the content of free monomers can be determined. But also the analysis of physical properties is possible. A typical application is the simultaneous monitoring of density and Melt Flow Index of Polyethylene. These parameters are crucial for the processing of the material, like extruding or moulding, making them the most frequently determined parameters in the quality control of polymers.

Instrumentation

Bruker Optics offers a wide variety of instrumentation to meet your specific needs. For process applications, the FT-NIR spectrometer MATRIX-F is recommended. Its multiplexing capability, ruggedness and easy serviceability make it the perfect process system. 

Various process measurement accessories are available for contact and non-contact measurements of liquids, solids and slurries. Near-infrared sample spectra can be collected from driers using diffuse reflectance probes or non-contact sensor heads. 

The use of fiber optics makes it possible to locate the instrument in either an enclosure in a hazardous location close to the measurement sites or in a control room. In a process environment the MATRIX-F can be used along with our process software CMET to perform the measurement and analysis of the sample and also output the results via a variety of I/O options (4-20mA, Modbus, Profibus DP, OPC DA etc).

4. Shimadzu: Measurement of Total Organic Carbon in SaltContaining Sediments

• Application note
• Full PDF for download

User Benefits:

• By performing a desalination process, it is possible to measure sediment samples containing salts.
• The measurement time for both TC and IC is approximately 6 to 8 minutes per analysis, allowing for rapid measurement.
• A single system enables TOC measurement for both liquid and solid samples.

Sediments refer to the surface-layer deposits accumulated at the bottoms of water bodies such as lakes, seas, and rivers. The organic matter in sediments plays various roles in aquatic ecosystems, including nutrient supply and pollutant adsorption. Therefore, measuring the organic matter content in sediments is crucial for understanding sediment characteristics and is an essential process for environmental management and ecosystem protection. Total organic carbon (TOC) measurement provides a quantitative evaluation of organic matter in sediments. 

However, when directly measuring sediments that contain salts, concerns arise regarding the influence of the salts on measurement values, as well as potential corrosion of the detector and other impacts on the equipment. To prevent these issues, a desalination process is required to reduce the salt concentration before measurement. 

This article explores sample pretreatment methods, including desalination, for salt-containing sediment samples and presents an example of TOC measurement in such sediments.

TOC Solid Sample Measurement System

The TOC solid sample measurement system (Fig. 1), consisting of a TOC-L combustion-type total organic carbon analyzer and an SSM-5000A solid sample combustion unit, quantifies carbon by detecting carbon dioxide (CO2) generated through combustion oxidation or acid decomposition of carbonates. 

For total carbon (TC) measurement, the sample is combusted at 900 °C in an oxygen atmosphere, allowing for the quantification of all carbon content within the sample. For inorganic carbon (IC) measurement, the sample is acidified with phosphoric acid and heated to 200 °C, extracting CO2 from carbonate-based carbon. TOC content is then determined as the difference between TC and IC values. 

The analysis is simple and quick—the sample is weighed into a sample boat and introduced into the system. To ensure accurate results, samples should be finely ground, as large particles may cause longer reaction times or incomplete reactions. 

Additionally, the TOC-L analyzer (Fig. 1, left) can also measure liquid samples (TOC, TC, IC) simply by adjusting the software settings.

Measurement Results

Examination of the Number of Desalination Treatments

The supernatant of the wet sample before desalination contained approximately 1.1 % chlorine. As desalination treatment was applied, the chlorine concentration in the supernatant gradually decreased. After two desalination treatments, the concentration dropped to below 200 ppm, and after three treatments, it fell to below 100 ppm. Based on these results, two desalination treatments were performed in this analysis, as shown in Fig. 5, before measuring both liquid and solid samples. The sample weight and supernatant volume used for calculations are also shown in Fig. 5. For volume conversion, pure water and supernatant were assumed to have a density of 1, meaning their weights were directly converted to volume. The reason why the volume of Supernatant (1) (35.7115 mL) was smaller than the amount of pure water added (40.4631 mL) is that during the first desalination treatment, some of the added pure water was absorbed by the dried sample.

TOC Loss Due to Desalination Treatment 

Table 3 shows the TOC concentration in the supernatants after desalination and the calculated TOC loss. An example of the measurement data is presented in Fig. 6. The presence of TOC in the supernatants confirms that TOC loss occurred during the desalination process, and this TOC loss amount is used for correction calculations of the TOC content in the dried sample.

Conclusion

This study examined appropriate pretreatment and desalination methods for TOC measurement of salt-containing sediment samples and determined the TOC values. 

The results confirmed that TOC loss occurred in the supernatants during desalination. To accurately determine TOC content, a correction calculation was performed by adding the TOC from both the supernatants and the desalinated dried sample. 

For the sediment sample used in this study, desalination by adding pure water and performing centrifugation proved to be an effective method. Applying the demonstrated desalination process enabled TOC measurement without salt interference. However, depending on sample properties and salt concentration, desalination conditions may require further optimization. (For salt-containing samples, the replacement interval for the detector and cell may be shorter than for normal samples.) 

This study suggests that the TOC solid sample measurement system is effective for TOC measurement in sediments. Furthermore, since the system allows for both liquid and solid TOC measurements by simply adjusting the software settings, it has great potential for applications in aquatic ecosystem studies.