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Compact NMR Spectroscopy in the field: A Versatile PAT Tool for Production of Specialty Chemicals
(2022)
Companies of chemical industry find themselves more often in a rapidly changing environment, e.g., due to variability of raw material quality or energy costs and efficiency. Process optimization and new process concepts become more and more important. For example, flexible and modular chemical plants can produce various high-quality products using multi-purpose equipment with short downtimes between campaigns and reduce time to market for new products. Intensified continuous production plants allow for difficult to produce compounds like exothermic reactions with high heat dissipation.
Therefore, fully automated “chemical” process control along with real-time quality control are prerequisites to such concepts and thus should be based on “chemical” information. A commercially available benchtop NMR spectrometer was integrated to the full requirements of an automated chemical production environment such as explosion safety, field communication, and robust evaluation of sensor data. Field studies in modular and conventional production plant setups show promising results gaining process knowledge for further optimization. NMR appeared as preeminent online analytical method and allow using a modular data analysis approach, which can even serve as reliable reference method for further calibration-dependent PAT applications (e.g., NIR spectroscopy). Based on experiences from these field studies an improved analyzer enclosure setup was developed and built, including the option of a secondary method besides NMR spectroscopy. Integrated control systems allow for a flexible implementation based on the available automation infrastructure at the chemical plant or pilot plant setup. In the future, fully integrated and intelligently interconnecting “smart” PAT systems and processes have the potential speed up the setup of production equipment for chemicals and pharmaceuticals and therefore help to reduce the time-to-market.
Chemical and pharmaceutical companies have to find new paths to survive successfully in a changing environment, while also finding more flexible ways of product and process development to bring their products to market more quickly – especially high-quality high-end products like fine chemicals or pharmaceuticals. A current approach uses flexible and modular chemical production units, which can produce different high-quality products using multi-purpose equipment with short downtimes between campaigns and reduce the time to market of new products.
NMR spectroscopy appeared as excellent online analytical tool and allowed a modular data analysis approach, which even served as reliable reference method for further Process Analytical Technology (PAT) applications. Using the available datasets, a second data analysis approach based on artificial neural networks (ANN) was evaluated. Therefore, amount of data was augmented to be sufficient for training. The results show comparable performance, while improving the calculation time tremendously. In future, such fully integrated and interconnecting “smart” systems and processes can increase the efficiency of the production of specialty chemicals and pharmaceuticals.
At the end of the article, ideas for solutions are discussed in order to speed up the implementation of new special products from the point of view of process analytics and to network the existing process chains more closely.
High-entropy alloys (HEAs) are innovative high-performance materials that have attracted more and more research attention. HEAs are characterized by a solid solution of typically five equiatomic metallic elements. In addition, medium-entropy alloys (MEA, with three elements) are of interest and become more and more important. Depending on the alloy concept, HEAs and MEAs show exceptional mechanical properties, especially high-strength and ductility combinations at both cryogenic and elevated temperatures combined with excellent corrosion resistance. Future structural HEA/MEA components can be exposed to potential applications with hydrogen containing environments like high-temperature water in pressurized nuclear reactors or aerospace structures. Other potential applications could be in materials for vessel walls in the field of cryogenic and high-pressure hydrogen storage. So far, the susceptibility of HEAs/MEAs to hydrogen assisted cracking (if any) and the hydrogen diffusion is not investigated in detail yet and can limit or extend possible applications of HEA/MEA as structural materials. In our work, we focused on the hydrogen absorption, diffusion, and distribution in a HEA (CoCrFeMnNi the original Cantor-alloy) and a MEA (CoCrNi). Cathodic hydrogen charging was carried out for the hydrogen ingress, and thermal desorption analysis (TDA) revealed complex hydrogen trapping in both alloy types up to 300 °C. The absorbed total hydrogen concentrations were > 100 ppm for the HEA and > 40 ppm for MEA. In addition, the assessment of the peak deconvolution is not trivial and must consider both experimental and microstructure influences.
The majority of ultrasonic devices used for non-
destructive testing in civil engineering require contact with the
surface of the concrete (specimen), which significantly increases
the time required for the measurement. This makes it impractical
for extensive investigation of large-scale structures such as bridge
decks, foundations, or tunnels.
In a pioneering approach, fluidic oscillators are used as contact
free ultrasonic sources to overcome the aforementioned limi-
tations. These robust and cost-effective actuators require only
pressurised air and are ideally suited for harsh environments. At
a constant supply pressure, they generate a continuous mono-
frequent actuation signal. Further, varying the supply pressure
via a fast pressure regulator was found to generate a frequency
modulated signal which enabled time-of-flight measurement with
an added advantage of increased signal to noise ratio. To
demonstrate the feasibility of this novel idea of non-contact
ultrasound, the results of the initial tests are presented.
The majority of ultrasonic devices used for non-destructive testing in civil engineering require contact with the surface of the concrete (specimen), which significantly increases the time required for the measurement. This makes it impractical for extensive investigation of large-scale structures such as bridge decks, foundations, or tunnels.
In a pioneering approach, fluidic oscillators are used as contact
free ultrasonic sources to overcome the aforementioned limitations. These robust and cost-effective actuators require only pressurised air and are ideally suited for harsh environments. At a constant supply pressure, they generate a continuous monofrequent actuation signal. Further, varying the supply pressure via a fast pressure regulator was found to generate a frequency modulated signal which enabled time-of-flight measurement with an added advantage of increased signal to noise ratio. To demonstrate the feasibility of this novel idea of non-contact ultrasound, the results of the initial tests are presented.
The majority of ultrasonic devices used for non-destructive testing in civil engineering require contact with the surface of the concrete (specimen), which significantly increases the time required for the measurement. This makes it impractical for extensive investigation of large-scale structures such as bridge decks, foundations, or tunnels.
In a pioneering approach, fluidic oscillators are used as contact free ultrasonic sources to overcome the aforementioned limitations. These robust and cost-effective actuators require only pressurised air and are ideally suited for harsh environments. At a constant supply pressure, they generate a continuous mono-frequent actuation signal. Further, varying the supply pressure via a fast pressure regulator was found to generate a frequency modulated signal which enabled time-of-flight measurement with an added advantage of increased signal to noise ratio. To demonstrate the feasibility of this novel idea of non-contact ultrasound, the results of the initial tests are presented.
Laser Induced Breakdown Spectroscopy – A Tool for Imaging the Chemical Composition of Concrete
(2022)
One of the most common causes of damage is the ingress of harmful ions into the concrete, which can lead to deterioration processes and affect structural performance. Therefore, the increasingly aging infrastructure is regularly inspected to assess durability. Regular chemical analysis can be useful to determine the extent and evolution of ion ingress and to intervene in a timely manner. This could prove more economical than extensive repairs for major damage, particularly for critical infrastructure. In addition to already established elemental analysis techniques in civil engineering such as potentiometric titration or X-ray fluorescence analysis, laser-induced breakdown spectroscopy (LIBS) can provide further important complementary information and benefits. The possibilities of LIBS are demonstrated using the example of a drill core taken from a parking garage.
One of the most common causes of damage is the ingress of harmful ions into the concrete, which can lead to deterioration processes and affect structural performance. Therefore, the increasingly aging infrastructure is regularly inspected to assess durability. Regular chemical analysis can be useful to determine the extent and evolution of ion ingress and to intervene in a timely manner. This could prove more economical than extensive repairs for major damage, particularly for critical infrastructure. In addition to already established elemental analysis techniques in civil engineering such as potentiometric titration or X-ray fluorescence analysis, laser-induced breakdown spectroscopy (LIBS) can provide further important complementary information and benefits. The possibilities of LIBS are demonstrated using the example of a drill core taken from a parking garage.
Whereas human factors (HF) in the non-destructive testing (NDT) of metallic components are a poorly investigated topic (in comparison to other industrial fields such as aviation), HF in the inspection of concrete components are even less known. Studies have shown that there is always some variability between individuals in their inspection results and that HF affect the reliability of NDT inspections. The aim of the ongoing WIPANO project is to draft a standard for a holistic reliability assessment, with concrete inspection as one case study. This includes also the HF. A human-oriented Failure Modes and Effects Analysis (FMEA) was carried out to do the following: a) identify possible human-related risks in tunnel inspection processes using a laser scan method (including data collection,evaluation, and assessment of tunnel damage) and b) evaluate these human-related risks as regards their possible causes, consequences and probability of occurrence – in addition with respect to existing and possible preventive measures. The results show that the causes for possible failures can lie within people, the physical environment, technology, organisation, and extra-organisational environment. Whereas current preventive measures rely mostly on the individual and quality management practices, there is potential for even larger improvement at the organisational and extra-organisational level. The FMEA results were also used to develop a quantification method to further understand the HF in tunnel inspection, which could possibly be included in the information into the overall reliability assessment. The usage of qualitative and quantitative data collected through the human-FMEA within the proposed quantification method shows promise that HF can be quantified and could offer broader understanding of HF influences on inspection in various industries
Wide-range X-ray scattering datasets and analyses for all samples described in the 2020 publication "Gold and silver dichroic nanocomposite in the quest for 3D printing the Lycurgus cup". These datasets are composed by combining multiple small-angle x-ray scattering and wide-angle x-ray scattering curves into a single dataset. They have been analyzed using McSAS to extract polydispersities and volume fractions. They have been collected using the MOUSE project (instrument and methodology).
Visually detecting irregularities on components is a complex process, influenced by physical, technical, and human factors. Current standards mainly focus on illuminance, demanding highest accuracy for it, without providing scientific justification. In this research, 63 inspectors visually inspected forgings, with and without crack-like indications. The influence of illuminance on probability of detection was investigated. Therefore, illuminance was varied in three steps (200 lx, 350 lx, 500 lx). Human factors (e.g., experience, motivation) were recorded by using questionnaires. The results show no significant difference in probability of detection between the three illuminance levels. Equal probability of detection rates could be achieved at illuminances below and at the required threshold (500 lx). A difference in illuminance was found between the measurement point and the test area of the respective participant. This leads to higher assumed illuminance than present on the component. Compared with the measurement accuracy of the used illuminance meter, none of these deviations could be used to explain the similar results at different illuminance. The fact that illuminance has a significant influence in detecting indications has been disproven for this case. Whether human factors can provide explanation for the results remains unclear. This will be investigated in further research.
Existing concrete structures were usually designed for lifetimes of several decades. The current and urgently required efforts to increase sustainability and protect the environment will likely result in extended service lives up to 100 years. To achieve such objectives, it is required to assess structures over their entire lifecycles. Non-destructive testing (NDT) methods can reliably support the assessment of existing structures during the construction, operational, and decommissioning phases. One of the most important and safety-relevant components of a prestressed concrete structure are the tendons. NDT methods such as the ultrasonic echo method are suitable for both the detection and the localization of the tendons, i.e., the measurement of their geometrical position inside the component. The uniqueness of structures, concrete heterogeneity, and varying amounts of secondary components such as the reinforcement represent obstacles in the application of these methods in practice. The aim of this contribution is to demonstrate a practicable procedure, that can be used in the field to determine the parameters required for the measuring data analysis without extensive knowledge about the investigated components. For this purpose, a polyamide reference specimen is used to show which steps are required to obtain reliable imaging information on the position of tendons from the measurement data. The procedure is then demonstrated on a concrete test specimen that covers various relevant and practice-oriented test scenarios, such as varying tendon depths and component thicknesses.
Each engineering decision is based on a number of more or less accurate information. In assessment of existing structures, additional relevant information collected with on-site inspections facilitate better decisions. However, observed data basically represents the physical characteristic of interest with an uncertainty. This uncertainty is a measure of the inspection quality and can be quantified by expressing the measurement uncertainty. The internationally accepted rules for calculating measurement uncertainty are well established and can be applied straightforwardly in many practical cases. Nevertheless, the calculations require the occasionally time-consuming development of an individually suitable measurement model. This contribution attempts to emphasize proposals for modelling the non-destructive depth measurement of tendons in concrete using the ultrasonic echo technique. The proposed model can serve as guideline for the determination of the quality of the measured information in future comparable inspection scenarios.
Contamination of the environment with antibiotics is of great concern as it promotes the evolution of antimicrobial resistances. In case of amoxicillin (AMX) in the aquatic environment, further risk arises from hydrolysis products (HPs) which can cause allergy. To assess these risks, a comprehensive investigation and understanding of the degradation of AMX is necessary. We investigated the hydrolysis rate of AMX in different types of water as well as the influence of temperature and irradiation. The content of the heavy metal ions copper and zinc was found to be crucial for the hydrolysis rate of AMX and stability of HPs. Eventually, a new degradation pathway for AMX could be elaborated and confirmed by tandem mass spectrometry (LC-MS/MS).
Whereas human factors (HF) in the non-destructive testing (NDT) of metallic components are a poorly investigated topic (in comparison to other industrial fields such as aviation), HF in the inspection of concrete components are even less known. Studies have shown that there is always some variability between individuals in their inspection results and that HF affect the reliability of NDT inspections. The aim of the ongoing WIPANO project is to draft a standard for a holistic reliability assessment, with concrete inspection as one case study. This includes also the HF. A human-oriented Failure Modes and Effects Analysis (FMEA) was carried out to do the following: a) identify possible human-related risks in tunnel inspection processes using a laser scan method (including data collection,evaluation, and assessment of tunnel damage) and b) evaluate these human-related risks as regards their possible causes, consequences and probability of occurrence – in addition with respect to existing and possible preventive measures. The results show that the causes for possible failures can lie within people, the physical environment, technology, organisation, and extra-organisational environment. Whereas current preventive measures rely mostly on the individual and quality management practices, there is potential for even larger improvement at the organisational and extra-organisational level. The FMEA results were also used to develop a quantification method to further understand the HF in tunnel inspection, which could possibly be included in the information into the overall reliability assessment. The usage of qualitative and quantitative data collected through the human-FMEA within the proposed quantification method shows promise that HF can be quantified and could offer broader understanding of HF influences on inspection in various industries.
Chemical and pharmaceutical companies have to find new paths to survive successfully in a changing environment, while also finding more flexible ways of product and process development to bring their products to market more quickly – especially high-quality high-end products like fine chemicals or pharmaceuticals. A current approach uses flexible and modular chemical production units, which can produce different high-quality products using multi-purpose equipment with short downtimes between campaigns and reduce the time to market of new products.
NMR spectroscopy appeared as excellent online analytical tool and allowed a modular data analysis approach, which even served as reliable reference method for further Process Analytical Technology (PAT) applications. Using the available datasets, a second data analysis approach based on artificial neural networks (ANN) was evaluated. Therefore, amount of data was augmented to be sufficient for training. The results show comparable performance, while improving the calculation time tremendously. In future, such fully integrated and interconnecting “smart” systems and processes can increase the efficiency of the production of specialty chemicals and pharmaceuticals.
In addition to already established structural monitoring methods such as deformation, inclination or strain gauges or acoustic emission sensors, sonic or ultrasonic monitoring might provide valuable information about the condition or alteration of a structure. Sensors such as geophones, recording ambient noise in the sonic and subsonic frequency range can provide information beyond modal analysis by using interferometric methods. Wave velocities determined by this method are related to the elastic properties and stiffness of material and structure and can be converted into damage indicators. Embedded active ultrasonic transducer networks can provide more detailed insight about deterioration or damages again, using interferometric technologies. This approach is extremely sensible, detecting relative change in velocity on down to 10-5. These methods, including benefits and remaining challenges, are demonstrated using data from a test structure at BAM’s test site demonstrating the case of prestress loss, and data from an actual bridge still under traffic.
Existing concrete structures were usually designed for lifetimes of several decades. The current and urgently required efforts to increase sustainability and protect the environment will likely result in extended service lives up to 100 years. To achieve such objectives, it is required to assess structures over their entire lifecycles. Non-destructive testing (NDT) methods can reliably support the assessment of existing structures during the construction, operational, and decommissioning phases. One of the most important and safety-relevant components of a prestressed concrete structure are the tendons. NDT methods such as the ultrasonic echo method are suitable for both the detection and the localization of the tendons, i.e., the measurement of their geometrical position inside the component. The uniqueness of structures, concrete heterogeneity, and varying amounts of secondary components such as the reinforcement represent obstacles in the application of these methods in practice. The aim of this contribution is to demonstrate a practicable procedure, that can be used in the field to determine the parameters required for the measuring data analysis without extensive knowledge about the investigated components. For this purpose, a polyamide reference specimen is used to show which steps are required to obtain reliable imaging information on the position of tendons from the measurement data. The procedure is then demonstrated on a concrete test specimen that covers various relevant and practice-oriented test scenarios, such as varying tendon depths and component thicknesses.