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In this article, we demonstrate a promising inline near-infrared measurement scheme for 24/7 biofilm monitoring based on cost-effective microelectromechanical system-based spectrometer technology. The shown near-infrared spectral data, acquired at a beer-canning line during a representative time span of 10 days, are analyzed by means of principal component analysis and the performance of the monitoring system and its capability to identify biofilms on its sensor surface are investigated by comparing spectral response with results of offline polymerase chain reaction measurements of smear samples. Correlations between presence of a biofilm and its thickness with scores on PC1 and PC2, respectively, were observed.

BackgroundThe primary aim of this study was to collect information on the surgical procedures used to implant two cochlear implant variants (non-pin and pin: Concerto and Concerto Pin from Med-El) in adults and children and to assess their medium-term stability. A secondary aim was to assess the safety of these variants, both of which permit a minimally invasive surgical protocol to be used. The pin variant has greater flexibility in positioning and fixing of the implant, with the pins ensuring implant stability; also it requires less or no drilling and no tie-down sutures.Materials and MethodsNon-pin and pin cochlear implant variants (Concerto and Concerto Pin from Med-El) were implanted in adults and children (n = 116) in 5 clinics. The different surgical techniques and methods of implant fixation were documented intraoperatively. Implant stability was subjectively assessed at first fitting and again approximately 3 and 6 months later. Safety was assessed based on the number and severity of adverse events.ResultsWith all non-pin variants suture fixation was always performed, but with the pin variant this was done for just 43% of adults and 49% of children (in the remainder, no additional fixation was performed). The study demonstrated the stability of both cochlear implant variants in children and adults, with no shifting or rocking observed. There were 33 adverse events reported during the study, 10 of which (9%) were classified as related to the device or procedure.ConclusionsImplant stability and safety can be achieved through various surgical techniques and fixation methods when implanting either the Concerto or Concerto Pin.

In this contribution, we present a high-speed, multiplex, grating spectrometer based on a spectral coding approach that is founded on principles of compressive sensing. The spectrometer employs a single-pixel InGaAs detector to measure the signals encoded by an amplitude spatial light modulator (digital micromirror device, DMD). This approach leads to a speed advantage and multiplex sensitivity advantage atypical for standard dispersive systems. Exploiting the 18.2 kHz pattern rate of the DMD, we demonstrated 4.2 ms acquisition times for full spectra with a bandwidth of 450 nm (5250–4300 cm−1, 1.9–2.33 µm). Due to the programmability of the DMD, spectral regions of interest can be chosen freely, thus reducing acquisition times further, down to the sub-millisecond regime. The adjustable resolving power of the system accessed by means of computer simulations is discussed, quantified for different measurement modes, and verified by comparison with a state-of-the-art Fourier-transform infrared spectrometer. We show measurements of characteristic polymer absorption bands in different operation regimes of the spectrometer. The theoretical multiplex advantage of 8 was experimentally verified by comparison of the noise behavior of the spectral coding approach and a standard line-scan approach.

In this contribution we present results on non-destructive chemical imaging in the mid-infrared (MIR) region of well-defined biofilms formed by Pseudomonas simiae. Biofilms were grown on stainless steel slides using a static biofilm model (incubation lasted for seven days at 10 °C, with repetitive medium changes). The MIR spectra correlate with fundamental molecular vibrations and are therefore characteristic for chemical composition and structure [1, 2]. Besides a brief insight into the systematic of how the investigated biofilms were grown the main focus will be on MIR spectroscopic measurements including dynamic observation of drying processes of bacteria, as well as spatially resolved scans of the steel plates with an MIR microscope. The obtained hyperspectral chemical images of biofilms were analyzed by various spectroscopic data analysis techniques. Furthermore, the dynamic spectroscopic observation of the drying process of planktonic Pseudomonas simiae cultures in nutrient solution gave insight in dynamic variances in certain functional chemical groups of the bacteria. These variances have also been observed in biofilm samples and may correlate with vitality. The MIR chemical images, where each pixel is composed of an entire MIR spectrum (4000-400 cm-1) provide detailed information of the investigated biofilms such as their composition and spatial structure. The overlay with conventional microscope images relates spectroscopic to visual data, both laterally resolved in the µm-range, over a scan area of up to 10 x 40 mm². The variation of the vibrational bands was screened, revealing high and low variance bands, to identify certain spectral regions suitable for classification of the investigated biofilm samples. Characteristic spectral bands were found and related to data from literature. Furthermore, differences in the spatial distribution of proteins and carbohydrates as part of the bacteria and extracellular polymeric substances were clearly identified. Acknowledgment: This work was created within a research project of the des Austrian Competence Centre for Feed and Food Quality, Safety and Innovation (FFoQSI). The COMET-K1 competence centre FFoQSI is funded by the Austrian ministries BMVIT, BMDW and the Austrian provinces Niederoesterreich, Upper Austria and Vienna within the scope of COMET -Competence Centers for Excellent Technologies. The programme COMET is handled by the Austrian Research Promotion Agency FFG. References:[1] Andreas Schwaighofer, Markus Brandstetter and Bernhard Lendl , “Quantum cascade lasers (QCLs) in biomedical spectroscopy”, Chem. Soc. Rev. 46, 5903-5924 (2017)[2] Jakob Kilgus, Gregor Langer, Kristina Duswald, Robert Zimmerleiter, Ivan Zorin, Thomas Berer, and Markus Brandstetter, "Diffraction limited mid-infrared reflectance microspectroscopy with a supercontinuum laser," Opt. Express 26, 30644-30654 (2018)

The physico-chemical properties of Melamine Formaldehyde (MF) based thermosets are largely influenced by the degree of polymerization (DP) in the underlying resin. On-line supervision of the turbidity point by means of vibrational spectroscopy has recently emerged as a promising technique to monitor the DP of MF resins. However, spectroscopic determination of the DP relies on chemometric models, which are usually sensitive to drifts caused by instrumental and/or sample associated changes occurring over time. In order to detect the time point when drifts start causing prediction bias, we here explore a universal drift detector based on a faded version of the Page-Hinkley (PH) statistic, which we test in three data streams from an industrial MF resin production process. We employ committee disagreement (CD), computed as the variance of model predictions from an ensemble of partial least squares (PLS) models, as a measure for sample-wise prediction uncertainty and use the PH statistic to detect hanges in this quantity. We further explore supervised and unsupervised strategies for (semi-)automatic model adaptation upon detection of a drift. For the former, manual reference measurements are requested whenever statistical thresholds on Hotelling’s $T^2$ and/or Q-Residuals are violated. Models are subsequently re-calibrated using weighted partial least squares in order to increase the influence of newer samples, which increases the flexibility when adapting to new (drifted) states. Unsupervised model adaptation is carried out exploiting the dual antecedent-consequent structure of a recently developed fuzzy systems variant of PLS termed FLEXFIS-PLS. In particular, antecedent parts are updated while maintaining the internal structure of the local linear predictors (i.e. the consequents). We found improved drift detection capability of the CD compared to Hotelling’s $T^2$ and Q-Residuals when used in combination with the proposed PH test. Furthermore, we found that active selection of samples by active learning (AL) used for subsequent model adaptation is advantageous compared to passive (random) selection in case that a drift leads to persistent prediction bias allowing more rapid adaptation at lower reference measurement rates. Fully unsupervised adaptation using FLEXFIS-PLS could improve predictive accuracy significantly for light drifts but was not able to fully compensate for prediction bias in case of significant lack of fit w.r.t. the latent variable space.

Recent developments in mid-infrared (MIR) spectroscopic ellipsometry enabled by quantum cascade lasers (QCLs) have resulted in a drastic improvement in signal-to-noise ratio compared to conventional thermal emitter based instrumentation. Thus, it was possible to reduce the acquisition time for high-resolution broadband ellipsometric spectra from multiple hours to less than 1 s. This opens up new possibilities for real-time in-situ ellipsometry in polymer processing. To highlight these evolving capabilities, we demonstrate the benefits of a QCL based MIR ellipsometer by investigating single and multilayered polymer films. The molecular structure and reorientation of a 2.5 µm thin biaxially oriented polyethylene terephthalate film is monitored during a stretching process lasting 24.5 s to illustrate the perspective of ellipsometric measurements in dynamic processes. In addition, a polyethylene/ethylene vinyl alcohol/polyethylene multilayer film is investigated at a continuously varying angle of incidence (0∘– 50∘) in 17.2 s, highlighting an unprecedented sample throughput for the technique of varying angle spectroscopic ellipsometry in the MIR spectral range. The obtained results underline the superior spectral and temporal resolution of QCL ellipsometry and qualify this technique as a suitable method for advanced in-situ monitoring in polymer processing.

Mid-infrared (MIR) supercontinuum (SC) lasers are an attractive new option in the field of IR spectroscopy, especially for standoff detection. Supercontinuum radiation unites high brightness, high spatial coherence, and broadband spectral coverage, thereby surpassing thermal IR sources and challenging quantum cascade lasers. The employed SC source operates in the spectral region of 1.2–4.6 µm, filling the spectral gap where quantum cascade lasers lack broader availability. In this work, the SC radiation was recorded by compact Fabry–Pérot filter spectrometers ideally suited for sensitive standoff detection with real-time capability. The noise performance of the setup and measurements of different substances at standoff distances are presented, e.g., of different paints on a metal surface and an explosive precursor. Furthermore, the real-time capability of the setup is demonstrated by monitoring the evaporation of liquid 2-propanol.

Fourier transform infrared (FT-IR) spectrometers have been the dominant technology in the field of mid-infrared (mid-IR) spectroscopy for decades. Supercontinuum laser sources operating in the mid-IR spectral region now offer the potential to enrich the field of FT-IR spectroscopy due to their distinctive properties, such as high-brightness, broadband spectral coverage and enhanced stability. In our contribution, we introduce this advanced light source as a replacement for conventional thermal emitters. Furthermore, an approach to efficient coupling of pulsed mid-IR supercontinuum sources to FT-IR spectrometers is proposed and considered in detail. The experimental part is devoted to pulse-to-pulse energy fluctuations of the applied supercontinuum laser, performance of the system, as well as the noise and long-term stability. Comparative measurements performed with a conventional FT-IR instrument equipped with a thermal emitter illustrate that similar noise levels can be achieved with the supercontinuum-based system. The analytical performance of the supercontinuum-based FT-IR spectrometer was tested for a concentration series of aqueous formaldehyde solutions in a liquid flow cell (500 µm path length) and compared with the conventional FT-IR (130 µm path length). The results show a four-times-enhanced detection limit due to the extended path length enabled by the high brightness of the laser. In conclusion, FT-IR spectrometers equipped with novel broadband mid-IR supercontinuum lasers could outperform traditional systems providing superior performance, e.g., interaction path lengths formerly unattainable, while maintaining low noise levels known from highly stable thermal emitters.

Optical coherence tomography (OCT) is a high-resolution three-dimensional imaging technique that enables non-destructive measurements of surface and subsurface microstructures. Recent developments of OCT operating in the mid-infrared (MIR) range (around 4 {\mu}m) lifted fundamental scattering limitations and initiated applied material research in formerly inaccessible fields. The MIR spectral region, however, is also of great interest for spectroscopy and hyperspectral imaging, which allow highly selective and sensitive chemical studies of materials. In this contribution, we introduce an OCT system (dual-band, central wavelengths of 2 {\mu}m m and 4 {\mu}m) combined with MIR spectroscopy that is implemented as a raster scanning chemical imaging modality. The fully-integrated and cost-effective optical instrument is based on a single supercontinuum laser source (emission spectrum spanning from 1.1 {\mu}m to 4.4 {\mu}m). Capabilities of the in-situ correlative measurements are experimentally demonstrated by obtaining complex multidimensional material data, comprising morphological and chemical information, from a multi-layered composite ceramic-polymer specimen., Comment: 12 pages, 9 figures

Miniature spectrometers based on microelectromechanical systems (MEMS) are a compact, cost-efficient and rugged alternative to conventional infrared spectrometers. Different practical applications of this emerging technology are presented to demonstrate its applicability in industrial process monitoring.

Novel types of supercontinuum sources radiating in the infrared (IR) spectral region provide ultra-broadband spectral coverage and maintain distinctive laser-like properties of emission such as brightness, spatial coherence and high power. Being a perfectly suitable light source for mid-infrared optical coherence tomography (OCT) and spectroscopy, supercontinuum sources initiated a significant amount of recent developments in these fields and promise to be a gamechanging factor in the nearest future. In this paper, we exhibit a simple, optimized and relatively cost-effective system operating in near and mid-infrared ranges and combining OCT and co-registered IR spectroscopy. The performance of the OCT modality of the setup is evaluated with respect to the sensitivity and roll-off. Due to reduced scattering inherited with the new spectral window, we achieve the enhancement in the penetration depth in artificial paintings, ceramics and pottery. Furthermore, the hyperspectral data is used to supplement structural information and access to the chemical composition of the sample. The gained results reveal the potential of the multimodal system for non-destructive testing, art and cultural objects diagnosis.

In this work, mid-infrared hyperspectral images of multilayer polymer film (MLPF) cross sections are acquired with a high-speed quantum cascade laser (QCL) based mid-infrared microscope and analyzed using different data analysis techniques. The investigated MLPF is a polypropylene (PP) and ethylene-vinyl alcohol co-polymer (EVOH) composite commonly used for food packaging due to its outstanding barrier characteristics. Pure band integration of supposedly selective absorption bands for the two constituents of the MLPF is compared to principal component analysis (PCA) and multivariate curve resolution (MCR) algorithms regarding the ability to spatially resolve the differently composed areas in the MLPF. While both pure band integration and PCA are strongly affected by common physical artifacts in the spectral data, such as sample tilt, scattering or interference effects, MCR managed to give a clear picture of the composition of the MLPF, which matches the actual situation given by the manufacturing process. The obtained results can guide the way to the application of high-performance mid-infrared spectroscopic instrumentation for spatially resolved polymer analysis by meaningful interpretation of hyperspectral image data.

In this paper, a hierarchical iterative control algorithm is proposed to optimally balance grid load (both voltage drop and current load) while meeting consumers power demand. The proposed control architecture is based on the assumption that a certain proportion of the consumers can predict their consumption profile and adapt their control strategies to fulfill power consumption constraints. It is assumed that a simplified model of the power grid and a prediction based on historical data for the consumption profile of passive consumers are available. Based on the consumers’ consumption profile predictions, the controller proposes constraints for predictively controlled buildings (PCBs) at critical times, so that these consumers can adapt their consumption strategies in advance. The control algorithm also deals with the case of noncompliant consumers. It has low-communication requirements and consumer information is only shared with the hierarchical controller. The method is verified by simulations of an existing power grid with two PCBs. For this purpose, a grid linearization method and a model predictive controller for a building are suggested.

Model predictive control (MPC) is highly suitable for building heating and cooling control because it exploits disturbance predictions, obeys constraints, and enables optimal building operation in terms of user comfort and energy efficiency. This work presents a highly efficient nonlinear modular MPC concept. It optimally controls both, heating and cooling activities in a low-energy office building simultaneously. Relevant system nonlinearities are considered through a nonlinear prediction model, an LTI MPC optimization step, and an efficient mixed-integer mapping to setpoint temperatures in the building. The involved optimization problems are efficiently solvable and enable realtime control, and the controller structure allows for retrofitting and can directly be incorporated into the existing building control infrastructure. A clear formulation of thermal user comfort and energy efficiency allows straightforward tuning. Excellent control performance and robustness are observed in detailed co-simulation studies, significantly outperforming a classical rule-based reference control law. Possible approaches to analyze robust stability of the controlled system are discussed and related to results of robust TS-fuzzy system analysis.

Mid-infrared hyperspectral imaging is advanced by the application of novel supercontinuum laser technology enabling short acquisition times and high SNR. Diffraction limited microscopic as well as macroscopic measurements at standoff distances are presented.

In this paper we present a multimodal OCT imaging system operating in the NIR and MIR spectral region. NIR/MIR Supercontinuum source based multimodal OCT provides new insights in scattering .materials. The system combines the modality of OCT and spectroscopy and enables a structural and specific characterization of different ceramics, polymers or composites.

We introduce a compressive sensing based approach for single pixel hyperspectral chemical imaging in a broad spectral range in the near-infrared. Fully integrated MEMS based Fabry-Pérot tunable filter spectrometers and a digital micro-mirror device were employed to achieve spectral and spatial resolution, respectively. The available spectral range from 1500 to 2200 nm covers molecular overtone vibrations enabling chemical identification. Hyperspectral images of different adhesives deposited on a textile were recorded revealing their chemical composition. Furthermore, spectrally resolved near-infrared images with compression rates up to 90% are presented. The approach of single pixel imaging illustrates a promising technology for the infrared spectral range superior to conventionally used costly focal plane arrays.

Recent developments and commercial availability of low-noise and bright infrared (IR) supercontinuum sources initiated intensive applied research in the last few years. Covering a significant part of near- and mid-infrared spectral ranges, supercontinuum radiation opened up unique possibilities and alternatives for the well-established imaging technique of optical coherence tomography (OCT). In this contribution, we demonstrate the development, performance, and maturity of a cost-efficient dual-band Fourier-domain IR OCT system (2 µm and 4 µm central wavelengths). The proposed OCT setup is elegantly employing a single supercontinuum source and a pyroelectric linear array. We discuss adapted application-oriented approaches to signal acquisition and post-processing when thermal detectors are applied in interferometers. In the experimental part, the efficiency of the dual-band detection is evaluated. Practical results and direct comparisons of the OCT system operating within the employed sub-bands are exhibited and discussed. Furthermore, we introduce the 2 µm OCT sub-system as an affordable alternative for art diagnosis; therefore, high resolution and sensitive measurements of the painting mock-ups are presented. Finally, potentials of the dual-band detection are demonstrated for lithography-based manufactured industrial ceramics.

In this contribution, we demonstrate the realization and application of a low-cost, flexible, small and fast hyperspectral imaging approach operating in the midinfrared fingerprint region where most molecules exhibit their fundamental vibrations. Following this approach, the recording of chemical images of macroscopic-sized samples at standoff distances in reflection geometry is possible. The optical setup is based on spectral identification by means of a MEMS-based Fabry-Pérot interferometer combined with 2D-snapshot spatial resolution using a bolometer camera. Results show the successful spatially resolved (resolution below 500 µm) chemical identification of different samples deposited on a metal surface (FOV = 6 × 5 cm) at a working distance of 35 cm.

Chemical mapping was demonstrated with a mid-infrared (MIR) microspectroscopy setup based on a supercontinuum source (SC) emitting in the spectral range from 1.55 to 4.5 µm and a MEMS-based Fabry-Perot filter spectrometer. Diffraction limited spatial resolution in reflection geometry was achieved. A multilayer film consisting of different polymers and mixtures thereof was measured and results were compared to those gained with a conventional FTIR microscope equipped with a thermal MIR source. Results show that compared to thermal sources, the application of the SC source results in higher signal-to-noise ratios together with better spatial resolution and faster scanning. Furthermore, diffraction limited imaging of red blood cells was demonstrated for the first time in the MIR spectral region in reflection mode. The distinctive characteristics of the MIR spectral region in conjunction with the high brightness, spatial coherence and broadband nature of supercontinuum radiation show the potential for improving infrared microscopy significantly.

A compact multi-bounce attenuated total reflection (ATR) probe combined with a Fabry-Perot filter spectrometer (FPFS) has been developed for detection of hydrogen peroxide used for oxidative gas scrubbing operating in the mid-infrared (MIR) spectral region. A novel MIR supercontinuum light source is employed to enhance the quantification capabilities of the sensor and is compared to a classical thermal emitter. An improvement of a factor of 4 in noise and approximately a factor of 3 in limit of detection is shown in this study allowing fast inline detection of aqueous hydrogen peroxide solutions around 0.1%.

Sulfur dioxide (SO2) trace gas detection based on quartz-enhanced photoacoustic spectroscopy (QEPAS) using a continuous wave, distributed feedback quantum cascade laser operating at 7.24 μm was performed. Influence of water vapor addition on monitored QEPAS SO2 signal was also investigated. A normalized noise equivalent absorption coefficient of NNEA (1σ) = 1.21 × 10−8 cm−1 W Hz−1/2 was obtained for the ν 3 SO2 line centered at 1,380.93 cm−1 when the gas sample was moisturized with 2.3 % H2O. This corresponds to a minimum detection limit (1σ) of 63 parts per billion by volume for a 1 s lock-in time constant.

Laser-based infrared spectroscopic ellipsometry (SE) is demonstrated for the first time, to the best of our knowledge, by applying a tunable quantum cascade laser (QCL) as a mid-infrared light source. The fast tunability of the employed QCL, combined with phase-modulated polarization, enabled the acquisition of broadband (900–1204 cm−1), high-resolution (1 cm−1) ellipsometry spectra in less than 1 second. A comparison to a conventional Fourier-transform spectrometer-based IR ellipsometer resulted in an improved signal-to-noise ratio (SNR) by a factor of at least 290. The ellipsometry setup was finally applied for the real-time monitoring of molecular reorientation during the stretching process of an anisotropic polypropylene film, thereby illustrating the advantage of sub-second time resolution. The developed method exceeds existing instrumentation by its fast acquisition and high SNR, which could open up a set of new applications of SE such as ellipsometric inline process monitoring and quality control.

We present the design and fabrication of a single-mode slab waveguide structure for mid-infrared spectroscopy optimized for broadband coupling. The sensor uses grating couplers for robust off-axis coupling and a silicon nitride guiding layer for mechanical robustness. An external cavity quantum cascade laser-based transmission method is introduced for characterizing the structure’s broadband coupling behavior. Light from an external cavity quantum cascade laser with a spectral range of 0.5 μm around 6 μm was coupled into the waveguide without the need for moving parts. First spectra taken with this sensor are presented.

The development of InGaAs based terahertz quantum cascade lasers is reported. This material system is an attractive alternative to the used GaAs/AlGaAs due the smaller effective mass. Using a symmetric quantum cascade design allows to understand the barrier interface and to realize high performance devices.

The emergence of new laser-based mid-infrared (MIR) sources, such as quantum cascade lasers (QCL), led to substantial developments in the field of MIR spectroscopy in the last decade. Recently, also MIR supercontinuum (SC) sources became available. They combine broadband spectral emission known from thermal sources emission with coherent properties known from laser sources like QCLs. Nevertheless, while the latter already find practical application in the field of optical sensing, SC sources have yet to prove their applicability. In this contribution we present the development, characterization and application of a measurement concept consisting of a fiber-coupled broadband MIR SC source (1.75 μm-4.2 μm, 75 mW optical power) and a fully-integrated MOEMS-based Fabry-Perot microspectrometer (FPMS) for MIR spectroscopy. The main hindrance for the use of SC sources in spectroscopy so far, are the significant pulse-to-pulse fluctuations arising from the non-linear nature of the SC generation process. We show to what extent spectral averaging makes sense and evaluate the noise performance. By combining a SC source and a FPMS it was possible to significantly reduce noise in spectral, time and polarization domain, resulting in a set-up suitable for MIR spectroscopy. The performance of the set-up was characterized both in transmission and reflection geometry. Low-noise absorption spectra of oils, polymers and aqueous solutions of acetic acid were acquired . Furthermore, time-resolved measurements of the curing process of ethyl-2-cyanoacrylate and results of the chemical mapping of a painted metal surface are reported. The obtained results prove the concept of SC-FPMS promising for MIR spectroscopy, characterized by its simplicity and versatility.

We present a multimodal optical setup, allowing non-contact photoacoustic imaging, optical coherence tomography (OCT), and non-contact mid-infrared photoacoustic spectroscopy. Photoacoustic signals are generated using a Nd:YAG laser and a tunable quantum cascade laser for photoacoustic imaging and spectroscopy, respectively. Photoacoustic signals are acquired by measuring the surface displacement of a specimen using a fiber-optic Mach-Zehnder interferometer. In the same fiber-optic network a spectral-domain OCT system is realized. Light from the photoacoustic detection laser and the OCT source are multiplexed into one fiber and the same objective is used for both imaging modalities. Light reflected from specimens is demultiplexed and guided to the respective imaging systems. To allow fast non-contact PAI and OCT imaging the detection spot is scanned across the specimens’ surface using a galvanometer scanner. As the same fiber-network and optical components are used for photoacoustic and OCT imaging the obtained images are co-registered intrinsically. Imaging is demonstrated on tissue mimicking and biological samples; spectral information is obtained for polystyrene and hemoglobin.

The presented investigations aimed to enhance surface sensitive infrared spectroscopy for chemical analysis by ultrasonic particle manipulation. The combination of these techniques has the potential for new measurement concepts for use in the chemical analysis of suspensions. Local increases of particle concentration brought about by ultrasound could facilitate measurements of molecular-specific infrared spectra of the suspending phase and particles independently. By changing the frequency of an ultrasonic standing wave around 2 MHz it was possible to control the position of particles in respect to the optically sensitive region of the infrared spectroscope. Results obtained with a set-up that enabled us to explore the application of an ultrasonic standing wave to push suspended particles at or into μm distances of the sensing element of an in-line fiber optic probe and subsequently retract them from there are presented. Light micrographs suggested, that the task was successfully accomplished with polystyrene beads suspended in methanol, aggregates were manipulated to and from the cut surface of the truncated, cone-shaped fibre probe tip by changes of the ultrasonic frequency between 1.85 and 1.87 MHz. Feasibility was confirmed by infrared absorption spectra recorded when PTFE particles suspended in tetrahydrofuran were used.

A novel approach for a physical chemosensor for liquids based on mid-infrared (mid-IR) laser spectroscopy is presented. Mid-infrared sensor systems access chemical information directly through measuring vibrational spectra of the samples under investigation. The introduction of mid-IR Quantum Cascade Lasers (QCLs) with their high spectral power density opens up new possibilities in liquid phase sensing. This concept is predestined for transmission measurements in highly absorbing matrices, such as aqueous phases. In a first step a pulsed ExternalCavity QCL (EC-QCL), tunable from 1030 – 1230 cm − 1 , was employed to perform transmission measurements of physiological solutions of path lengths > 125 μ m , thus significantly improving measurement capabilities of mid-IR sensors employing thermal light sources. Furthermore, the signal-to-noise ratios achieved compete with those obtainable with state-of-the-art FT-IR spectrometers. Results on direct determination of glucose and lactate in aqueous solutions are reported.

During the production process of beer, it is of utmost importance to guarantee a high consistency of the beer quality. For instance, the bitterness is an essential quality parameter which has to be controlled within the specifications at the beginning of the production process in the unfermented beer (wort) as well as in final products such as beer and beer mix beverages. Nowadays, analytical techniques for quality control in beer production are mainly based on manual supervision, i.e., samples are taken from the process and analyzed in the laboratory. This typically requires significant lab technicians efforts for only a small fraction of samples to be analyzed, which leads to significant costs for beer breweries and companies. Fourier transform mid-infrared (FT-MIR) spectroscopy was used in combination with nonlinear multivariate calibration techniques to overcome (i) the time consuming off-line analyses in beer production and (ii) already known limitations of standard linear chemometric methods, like partial least squares (PLS), for important quality parameters Speers et al. (J I Brewing. 2003;109(3):229-235), Zhang et al. (J I Brewing. 2012;118(4):361-367) such as bitterness, citric acid, total acids, free amino nitrogen, final attenuation, or foam stability. The calibration models are established with enhanced nonlinear techniques based (i) on a new piece-wise linear version of PLS by employing fuzzy rules for local partitioning the latent variable space and (ii) on extensions of support vector regression variants (𝜖-PLSSVR and ν-PLSSVR), for overcoming high computation times in high-dimensional problems and time-intensive and inappropriate settings of the kernel parameters. Furthermore, we introduce a new model selection scheme based on bagged ensembles in order to improve robustness and thus predictive quality of the final models. The approaches are tested on real-world calibration data sets for wort and beer mix beverages, and successfully compared to linear methods, showing a clear out-performance in most cases and being able to meet the model quality requirements defined by the experts at the beer company. Figure Workflow for calibration of non-Linear model ensembles from FT-MIR spectra in beer production .

Mid-infrared spectroscopy has been successfully applied for reagent-free clinical chemistry applications. Our aim is to design a portable bed-side system for ICU patient monitoring, based on mid-infrared absorption spectra of continuously sampled body-fluids. Robust and miniature bed-side systems can be achieved with tunable external cavity quantum cascade lasers (EC-QCL). Previously, single EC-QCL modules covering a wavenumber interval up to 250 cm-1 have been utilized. However, for broader applicability in biomedical research an extended interval around the mid-infrared fingerprint region should be accessible, which is possible with at least three or four EC-QCL modules. For such purpose, a tunable ultra-broadband system (1920 - 780 cm-1, Block Engineering) has been studied with regard to its transient emission characteristics in ns time resolution during different laser pulse widths using a VERTEX 80v FTIR spectrometer with step-scan option. Furthermore, laser emission line profiles of all four incorporated EC-QCL modules have been analysed at high spectral resolution (0.08 cm-1) and beam profiles with few deviations from the TEM 00 spatial mode have been manifested. Emission line reproducibility has been tested for various wavenumbers in step tune mode. The overall accuracy of manufacturer default wavenumber setting has been found between ± 3 cm-1 compared to the FTIR spectrometer scale. With regard to an application in clinical chemistry, theoretically achievable concentration accuracies for different blood substrates based on blood plasma and dialysate spectra previously recorded by FTIRspectrometers have been estimated taking into account the now accessible extended wavenumber interval.

We present a silicon (Si) based infrared (IR) absorption sensor which is suitable for integration into a miniaturized sensor system. The sensor is designed to operate in the wavelength region around λ=5 μm. We particularly discuss the design, the modeling and the optical characterization of the used materials. The sensor operates as a singlemode Si waveguide (WG) on low refractive index Si 3 N 4 membrane. The single-mode requirement for the WG is needed to avoid losses due to imperfections on the WG walls causing redistribution of the carried energy among the different modes. The waveguide interacts with the sample by means of the evanescent field which extends into the sample. This sensor configuration is not only compatible to the Si technology, but can also be realized on a single chip. In addition, the principle of operation is not limited to a single wavelength: by changing the waveguide dimensions, it can be applied to a broad spectral range. Thus, by its dimensions, performance and Si-compatibility, the sensor is expected to overcome previously published device concepts. The single-mode requirements lead to WG dimensions of 2 μm width x 600 nm height for an operation at λ=5 μm, which are verified by 3D simulations. For those parameters, the WG will support one transverse electric (TE) mode and one transverse magnetic (TM) mode. Efficient guidance is only obtained for the fundamental TE and TM modes. As an example, it is shown that mode TE1 is a non-guided mode. The experimentally obtained WG dimensions are 605 nm height and 2 μm width. In our paper we discuss issues with the design, the material characterization and first experimental results obtained with the recently fabricated prototypes.

Recent advances in combining ultrasonic particle manipulation with attenuated total reflection infrared spectroscopy of yeast suspensions are presented. Infrared spectroscopy provides highly specific molecular information about the sample. It has not been applicable to in-line monitoring of cells during fermentation, however, because positioning cells in the micron-thin measurement region of the attenuated total reflection probe was not possible. Ultrasonic radiation forces exerted on suspended particles by an ultrasonic standing wave can result in the buildup of agglomerates in the nodal planes, hence enabling the manipulation of suspended cells on the microscopic scale. When a chamber setup and a prototype in-line applicable probe were used, successful control over the position of the yeast cells relative to the attenuated total reflection sensor surface could be proven. Both rate of increase and maximum mid-infrared absorption of yeast-specific bands during application of a pushing frequency (chamber setup: 1.863 MHz, in-line probe: 1.990 MHz) were found to correlate with yeast cell concentration.

After providing an overview on the state-of-the-art of measuring condensed phase samples by quantum cascade lasers (QCL), this presentation will focus on protein analysis. The qualitative analysis of mid-IR spectra of aqueous protein solutions provides information on the secondary structure elements present in the proteins under study. In this work an external cavity (EC)-QCL was used for performing transmission measurements of different aqueous protein solutions in a CaF 2 flow cell with optical paths up to 75 μm. The strong temperature dependence of the v 2 -band of water overlapping the amide I absorption band (∼1650 cm−1) required a temperature stability of +/− 0.005°C. Successful determination of the secondary structures of albumin and β-lacto-globulin was achieved in the low g/L concentration range.

A portable point-of-care sensor employing a broadly tunable External Cavity Quantum Cascade Laser was applied for clinical multianalyte detection in human blood plasma. Glucose, triglyzerides, total protein, albumin, cholesterol and fibrinogen could be succesfully quantified.

Optical technology in the mid-infrared wavelength range is currently a rapidly developing field initiated by the availability of novel high-power and spatially coherent sources. Non-destructive testing techniques based on these sources are very promising for industrial and medical applications. However, there are still many engineering problems due to the technical challenges and high prices of the optical elements suitable for the mid-infrared region. In this paper, we report the development and performances of the first mid-infrared Fourier-domain optical coherence tomography based on a supercontinuum source and low-cost pyroelectric detector. The system is designed to operate in the spectral region around 4 μm. Experimental results are demonstrated for detections of embedded microstructures in ceramic materials and subsurface oil paint layers.