IRIS Technology presents its solutions at Expoquimia 2023

Raman Process Analyzer Visum Raman In-Line™ analyzing

Raman Process Analyzer: Innovation in Industrial Process Control

Innovation 4 December 2024

Real-time monitoring of free lacticide during the production of PLA (polylactic acid)

Monitoring of free lacticide levels during PLA (polylactic acid) production in real-time.

Reactive extrusion - REX

Reactive extrusion (REX) is a method of chemically modifying polymers during the extrusion process to improve their properties. Combining reaction and extrusion means taking advantage of the synergistic effects of shear forces and temperature to complete the reaction in less time, while the product is obtained directly in its final form.

One of the advantages of reactive extrusion is that the reactions are carried out without solvents or with a minimal amount compared to traditional batch polymerization processes. The result is a considerable reduction in costs and emissions, which makes the process more sustainable.

However, since each reactive extrusion process involves several characteristics, such as extruder geometry, screw speed, temperature profile, as well as the ratio and feed rate of the reactive species, which, in turn, are closely related to the throughput and residence time, the process is particularly complex and usually cannot be adequately modelled in terms of simple recipes or simple manufacturing rules.

Polylactic acid (PLA)

^{PLA structural unit}

Polylactic acid is a monomer used for the synthesis of PLA and is a bioplastic, i.e. bio-based and biodegradable, obtained from the anaerobic fermentation of renewable food sources and has numerous applications in the compostable packaging industry, its use as a filament in 3D printing and in the medical or surgical industry. It is also a rigid thermoplastic that can be semi-crystalline or fully amorphous, depending on the purity of the stereoisomer.

Visum NIR In-Line Probe™ as a control tool to monitor PLA synthesis by reactive extrusion

The use of analytical tools based on NIR spectroscopy provides a source of real-time information about what happens inside the reactive extruder during the L-lactide Ring Opening Polymerisation (ROP) process.

In this case, the most important source of information is the amount of L-lactide that has not reacted or polymerised during the process. Both the purity and the yield in terms of molecular weights as well as the mechanical and thermal properties of the product are highly dependent on the efficiency of the process.

Visum NIR In-LIne Probe™ monitoring of free lacticide

^{Visum NIR In-Line Probe™ monitoring PLA synthesis in ROP process}

The process analyser Visum NIR In-Line Probe™ -designed, manufactured and marketed by IRIS Technology Solutions, S.L.- (Spain) has been successfully used to monitor the polycondensation reaction of lactic acid that normally takes place at temperatures above 180 °C.

Unlike its sibling Visum NIR In-Line™ analyser, the Probe version has been specifically designed to work in even more aggressive environments using transmittance, reflectance or transflectance optical probes depending on the characteristics of the matrix to be monitored and the particular process conditions such as temperature, viscosity, pressure and explosion risk.

To monitor the reaction, a reflectance probe was used, attached to a reactor port suitably machined for this purpose.

As can be seen below, the predicted lactide concentration values have an RMSEP of 1.6% w/w when compared to the reference laboratory analysis, which is a more than acceptable uncertainty because the typical amount of lactide remaining is between 5 and 10%. The alternative, off-line analysis by chromatography (HPLC) could involve a waiting time of about 1 day, which is not suitable for any efficient process control task.

The ultimate goal is to optimise the residence time in the reactor: the shorter the better, as long as the concentration of remaining lactide (which has not polymerised) is kept low enough to guarantee the quality and purity of the final product. Incorrect extrusion settings result in loss of time, energy and raw materials, as the process is not reversible.

Machine learning predictive model metrics and regression lines. Grey dots represent modelling (“training”) spectra, while red dots represent validation spectra, which have not been included in the training set. Ordinates: Predicted L-lactide concentrations. Abscissae: Reference L-lactide concentrations provided by the traditional (HPLC) method.

In relation to the machine learning model, using the Model Builder of the proprietary Visum Master™ software, a non-expert user can easily create tailor-made calibrations as long as some reference spectra and the respective analyte concentrations are available. Since the Model Builder works according to AI heuristics, the best combination of mathematical pre-treatments and machine learning algorithms is found automatically without any input from the user. This means that the user could extend the applicability of the online analyser to a wider range of future applications beyond the specific case of PLA manufacturing.

In summary, since the Visum NIR In-Line Probe™ analyzer can acquire and mathematically process a representative spectrum in a fraction of a second, the entire reactive extrusion process can be automatically inspected in terms of the remaining amount of L-lactide so that the user can make real-time decisions on the updated optimal parameters.

By IRIS Technology Solutions

NIRS analysis of Brix degrees in whole apples in real time

Real-time cooking degree monitoring of gummies with Visum Raman In-Line™

Innovation 7 October 2024

Water Activity Analysis in animal feed with Visum Palm™ portable NIR

The water content in animal feed is a critical factor in feed quality and safety. Water is not only essential for the biological functions of animals, but also plays a crucial role in feed stability during storage, preservation, microbial activity, and food safety. Moisture, or more specifically water activity (Aw), directly influences the stability of the product and the likelihood of reactions affecting its quality.

In this paper we present the analysis of water content in animal feed by real-time infrared spectroscopy with the Visum Palm™ handheld analyser property of IRIS Technology Solutions SL.

Water Activity Analysis in animal feed

Water activity (Aw) is a more accurate measure than moisture content for predicting microbiological stability and feed shelf life. Water activity is defined as the ratio of the vapour pressure of water in the feed to the vapour pressure of pure water at the same temperature. It is expressed on a scale from 0 to 1, where 1 indicates the presence of pure water.

In animal feeds, the typical Aw value is typically in the range of 0.2 to 0.7 for dry products, which allows for greater stability during storage. When the water activity is higher than 0.7, the growth of microorganisms such as moulds and pathogenic bacteria is facilitated.

Thus, keeping water activity below 0.70 is crucial to prevent microbial growth and ensure feed safety.

Water Activity Analysis in animal feed with Visum Palm™

^{Left: Resultant regression curve for Aw – calibration samples (grey) and validation samples (blue) Right: Fisher-Pitman permutation test to determine the risk of overfitting the Aw model.}

Traditional Analysis Method

The most common traditional method in the industry for measuring the water content in animal feed is oven drying. This procedure involves the following steps:

Feed sample: A specified amount of sample is extracted and weighed.
Drying: The sample is placed in an oven at a constant temperature (usually between 105°C and 110°C) for a certain period of time (usually between 2 and 4 hours).
Calculation of water content: At the end of drying, the sample is reweighed and the weight loss is calculated as the amount of water evaporated.

This method is widely used due to its accuracy and simplicity, although it is time-consuming, labour-intensive in terms of sampling.

Determination of water activity with NIRS in seconds

For the development of the predictive model for water activity determination, we worked closely with a Mexican pet food manufacturer. A total of 345 calibration samples in the 0.1 – 1 % Aw range were used, of which 20% were automatically separated by the Model Builder Visum Master™ software for internal validation of the NIRS method.

As the processing of the data (spectra and laboratory references) is fully automated, the software itself executes and applies the most convenient processing routine and parameterisations according to the input data. At the end, it automatically applies a permutation test to check that the resulting model is useful for analysing future samples and that it is not the product of overfitting, which is also known as overfitting risk, an indicator of confidence in the analytical method.

As a result, the model developed to predict water activity in animal feed yielded a correlation coefficient (R²) of 0.96 and an RMSEP (root mean squared error of prediction) of ± 0.04. This validates the use of the Visum Palm™ portable NIR analyser as a real-time (< 3 seconds) method to determine water activity in feed and animal feed as a much more efficient alternative to the traditional method.

Importance of Water Content Analysis for Food Safety

Controlling water content and water activity in animal feed is essential for food safety for several reasons:

Prevention of microbial growth: Microorganisms need free water to grow and reproduce. If moisture content and Aw are too high, this facilitates the growth of pathogens such as Salmonella, E. coli and moulds, which can cause disease in both animals and humans, as they are linked to the food chain.
Product preservation: A feed with controlled water activity has a longer shelf life. Microbial growth and chemical reactions that cause nutrient deterioration are minimised when Aw is in optimal ranges.
Toxin control: Poor management of water content can allow the appearance of fungal toxins, such as aflatoxins, which can be highly hazardous to animals and thus to the human food chain.
Maintenance of nutritional quality: An adequate moisture level ensures that the nutrients present in the feed remain stable. Fat oxidation and vitamin degradation are accelerated in high moisture conditions, which reduces the nutritional quality of the feed.
Costs and efficiency: Controlled water content reduces economic losses, as the feed will have better stability during transport and storage, reducing the risk of losses due to contamination or spoilage.

Conclusions of analysis of water activity in animal feed

^{Visum Palm™ handheld or laboratory analyser}

Controlling water content and water activity in animal feed is vital not only to maintain the nutritional quality of the feed, but also to ensure food safety and prevent risks associated with microbial growth and contamination.

Traditional methods of analysis such as oven drying provide essential tools to keep these factors under control but are resource and time intensive compared to water activity analysis using NIRS infrared spectroscopy.

The portable Visum Palm™ analyser is capable of predicting Aw in feed samples in less than 3 seconds with an accuracy of ± 0.04, contributing to proper management of water activity during the production process, which is key to ensuring feed quality, animal health and sustainability of food production. As a handheld or benchtop (laboratory) multiparametric analyser, it can be used simultaneously to determine moisture, fat and fibre content, to mention the most important parameters in the production of pet food, thus constituting a fundamental tool for efficient analytical and product controls, even for agri-food raw materials.

By IRIS Technology Solutions

Real-time cooking degree monitoring of gummies with Visum Raman In-Line™

Jelly sweets, also called jelly candies, jelly beans, jelly fruit candies or gummies, are a broad category of chewy jelly-based candies that have been popular around the world for more than a century and more recently also include vitamins in their recipes for the production of healthy candies.

Depending on the recipe, gummies are made from starch, pectin, gelatin, glucose syrup, sugar, water, sodium citrate, fruit and plant extracts, flavourings, colourings and other additives, all of these ingredients are mixed together and various characteristics are controlled to obtain the best taste and texture. In order to meet these requirements, a critical factor during the production of gummy dough is the degree of starch gelatinisation and therefore a critical factor is to analyse the residual starch after the cooking process.

Level of starch cooking: the gelatinisation process

To achieve the gelatinisation of the gummy mass, starch is often used, of which potato and corn starch are the most popular and are available in a width range of modifications.

Gelatinisation, or ‘cooking’, is the process by which the starch granules are subjected to the action of water and temperature, which breaks the hydrogen bonds and dissolves the granules into the candy mass. After being subjected to a subsequent depositing and drying process, the final texture and consistency of the gummy is obtained.

In the confectionery industry, gelatinisation usually takes place in continuous cooking systems

Traditional analysis

At present, there is no inline method to monitor the degree of cooking continuously during production. Although there are several methods to determine the degree of cooking, they are all based on taking samples and analysing them off-line. This technique is labor intensive and requires qualified personnel, in addition to the difficulty it poses to make decisions and be able to correct process parameters in real time and thus avoid soft gummies, with an incorrect texture or subsequent problems in the demoulding process.

One of the methods used to control the end point of the cooking process is carried out in the laboratory using the technique of counting starch granules with a polarised light microscope.

This technique consists of the visual counting of starch particles and, depending on the quantity of particles present in the sample, the analyst can determine whether the cooking has been satisfactory or whether it is necessary to modify process parameters (temperature) or extend the cooking time. If the number of starch granules in the sample is less than or equal to 10, the degree of cooking is considered to be adequate, whereas if the number is higher, the degree of cooking is considered to be insufficient.

_{Starch granules under the polarised light microscope with the area marked in red for counting.}

Real-time cooking degree monitoring of gummies

A partnership for the future of the industry

IRIS Technology Solutions SL, a leading Spanish manufacturer of spectroscopy-based solutions for the control and monitoring of industrial processes, in collaboration with the Dutch manufacturer Tanis Confectionery B.V., a worldwide manufacturer of machinery for the production of gummies, have teamed up to develop a real-time method for monitoring the starch gelatinisation and thus offer an alternative, value-added solution to the entire industry.

Within this framework of collaboration, tests have been carried out for months in the facilities of the Tanis Innovation Center (The Netherlands) using the Visum Raman In-Line™ analyser property of IRIS Technology Solutions SL.

Raman spectroscopy is an analytical technique used to observe vibrational, rotational and other low-frequency modes in a system. It relies on the inelastic scattering of monochromatic light, a laser, to provide detailed information on molecular vibrations and chemical composition. Unlike NIR spectroscopy, it is particularly suitable for monitoring aqueous matrices or for determining the concentration of an analyte dissolved in water.

This technology is a non-invasive analytical technique that analyses in real time the product flow, in this case the gummy dough, by inserting a food grade immersion probe, capable of providing real time results of what is happening in the process with the appropriate calibration

Developing a real-time analytical method

During the test phase, different recipes based on potato starch, corn starch and with a combination of gelatin with starch were manufactured and monitored and cooked at different temperatures to obtain different degrees of starch gelatinisation during the cooking process in order to develop the cooking level prediction algorithm (adequately cooked / undercooked).

While the Visum Raman In-Line™ analyser was acquiring spectra throughout the cooking process of the different batches or recipes, samples were extracted and analysed by the reference method of visual counting using polarised light microscopy.

For the monitoring of the continuous process, the model was developed to determine two final classifications, “Adequately cooked” (≤10 starch granules) and “Undercooked” (>10 starch granules). The result obtained is the outcome of 3 consecutive analyses to confirm the degree of gelatinisation and to avoid any misclassification.

_{Left: comparison of the average pre-processed Raman spectrum of the different recipes used. Right: classification results of the model for five of the recipes. The points above the red dotted line correspond to measurements classified as adequately cooked.}

Conclusions

From the tests carried out, it could be concluded that the same predictive model can be used to make cooking level predictions for both corn and potato starch-based recipes.

For all batches made from both potato and corn starch the Visum Raman In-Line™ correctly classified their cooking level.

Next to the developed models it is possible to create unique models for unique candy recipes and ingredients with this inline method.

For the recipes with gelatin or modified starch that were analysed, more significant spectral differences were observed, so specific classificatory predictive models were performed for these formulations with similar validation results.

It is therefore possible to successfully predict the cooking level of both corn and potato starch-based jelly bean dough as well as different modified gelatines with the real-time raman process analyser, a truly more efficient alternative to the traditional and current method of analysis.

Key features of the Visum Raman In-Line™ Process Analyser

Sensor ready for use after switch-on (no warm-up required).
Analyser designed to operate in industrial environments.
Computer and embedded operating system.
785 nm laser excitation source.
Internal cooling system stable at -40°C.
IP 65-68.
Connection to the process via a food grade immersion probe.
Compatible with different communication drivers with PLC or SCADA of the plant.
It can be easily integrated in any position of the pipe.
Low-maintenance device.
With the Visum Master™ SMART version software, the user has an AI-supported Model Builder for developing, adjusting or updating predictive models for different recipes or formulations.

^{Visum Raman In-Line™ process analyser}

By IRIS Technology Solutions

Plastic identification, verification and classification using Visum Palm™

identificación, verificación y clasificación

Plastic identification, verification and classification using Visum Palm™

In this article we will address the problem of classification and plastic identification using the Visum Palm™ handheld NIR analyser as an agile, real-time and non-destructive technique useful in different processes, whether in the recycling of post-industrial plastic, in the analysis and classification of post-consumer plastic, in the identification of polymeric raw materials for their industrialisation, or even in areas of research and development of new plastic.

In all these cases, near infrared spectroscopy is presented as a valuable tool used for the characterisation of plastic compared to traditional methods of analysis.

Identification and sorting is important in plastic recycling and in manufacturing when using recycled plastic, as in both cases it must be ensured that the plastic materials are as pure and clean as possible because low levels of impurities can significantly affect the quality and performance of a recycled batch.

Although there are several portable NIR analyzers on the market, it is important to consider the spectral range that the equipment works with, the size of the measurement area (spectrum acquisition) and the spectral resolution (the quality of the spectrum obtained). The new Visum Palm™ analyser has a measuring area of 10 mm diameter, operates in the spectral range 900-1700 nm with a resolution of only 3 nm (↓ nm = ↑ spectral resolution). It is a self-contained device with an embedded computer and touchscreen and therefore does not need to be connected to a computer or smartphone to work with it.

Análise de forragens e espectroscopia nir

The new Visum Palm™, which includes a polymers library, allows readings and determinations to be made at the line without the need for sample preparation in less than 3 seconds. It is also possible to use it as a laboratory device as it has a support base that allows the attachment of different sample holders for the analysis of pellets, flakes or plastic up to 2 mm.

The factory library included in the analyser has the following classes: PMMA, PE, PC, PETG, EVA, PVC, PET, PU, PS, ABS, PA, PP, VIN, PLA, PBT, PMP, POMC, PPS, PVA, PPSU, EMA, PHBV, PAEK, PBAT, PBS, TPES, TPS, MABS, HIPS, MBS, SBC, PCL, PEEK, PHB, SAN, PI, PB.

Extend and develop your own library with Visum Master™

Visum Master™ is a computer software that allows the end user to create, extend and strengthen their own identification, classification and quantification methods or libraries without the need for a specialist or technical knowledge of spectroscopy, making the analyser a truly open system to meet present and future analysis needs (new polymer classes, new suppliers, etc.).

As shown below, it is possible to incorporate spectra of new samples within an existing class or to incorporate new classes and thus keep the library as robust and up-to-date as possible in order to be able to classify or identify plastic.

Plastic identification

It is a working method that allows the plastic identification analysed within the library available in the analyser. The result obtained, as can be seen below, is the type of polymer with the highest similarity and the following (from highest to lowest similarity).

_{Image 1: Visum Palm™ screen performing plastic identification}

Plastic identification screen visum palm

Polymer Verification

As with plastic identification, it is based on a mathematical procedure of similarity but it allows choosing a type of material to be analysed within the identification library to confirm its identity. The result of the verification analysis is PASS / FAIL. In case of a negative result (FAIL), it provides the class corresponding to the type of plastic analysed. Both cases are shown below.

Plastic classification

In contrast to plastic identification analysis, classification uses machine learning algorithms to accurately analyse and classify samples that are spectrally very similar to each other, where a double check is necessary to determine the polymer class (PET/PETG, for example). Through the Visum Master™ software, the user can create his own classification libraries for the most problematic cases.

As a result of the analysis, the user obtains the corresponding class.

In conclusion, NIR spectroscopy is a very valuable and effective tool for plastic identification or classification and, although not covered in this article, it is also useful for manufacturers of plastic and new formulations to quantify blends. The open nature of the analyser through the Visum Master™ software makes the Visum Palm™ analyser an open, self-contained system that can continuously introduce new samples, spectra and generate different libraries without the need for a specialist.

By IRIS Technology Solutions

IRIS Technology Solutions at Alimentaria FoodTech 2023

At the end of September, IRIS Technology Solutions presented at Alimentaria FoodTech trade show 2023 Barcelona the various real-time quality and process control solutions for the industry that the Catalan company manufactures and markets under the Visum® brand.

Alimentaria-FoodTech is the machinery, technology and ingredients show that integrates the food processing and preservation value chain. It is a transversal fair that serves the food and beverage production industry from raw materials to commercial distribution.

Visum® Solutions

Visum® solutions optimize and digitize quality control on different production lines. They operate on the basis of NIR, Raman, Hyperspectral and Machine Vision spectroscopy, providing real-time information for decision making and rectification of production processes. In addition, trade show participants were able to see first-hand the new Visum Palm™ handheld NIR analyser.

The new Visum Palm™ analyzer has an innovative and ergonomic design, as well as the possibility to perform analysis at any time and place without the need to connect it to any external electronic device. This is possible because it incorporates an embedded touch screen and computer, which allow all the routine functionalities of the device.

In addition, it has the Visum Master™, this software, unlike the most common modeling and calibration software on the market, with which the user has to have certain technical knowledge about chemometrics or entrust such a task to a third party.

It allows to perform calibrations in an automated and agile way only by incorporating spectra and references (quantitative or qualitative), in addition to other functionalities.

Shealthy Project

IRIS Technology Solutions has also presented at FoodTech the European SHEALTHY project, which seeks to evaluate and develop an optimal combination of non-thermal sanitization, preservation and stabilization methods to improve safety (inactivation of pathogens and spoilage microorganisms) while preserving nutritional quality (up to 30%) and extending shelf life (up to 50%) of F&V products. By combining and modulating non-thermal technologies with minimal processing operations, SHEALTHY’s approach will finally be able to meet today’s growing consumer demand for healthy food.

By IRIS Technology Solutions

New Visum Palm™ AI-assisted handheld NIR analyser

IRIS Technology Solutions introduces the latest version of its Visum Palm™ portable NIR analyser to complement its Visum® range of real-time process analysers for industry.

The new Visum Palm™ is a fully portable NIR spectrophotometer that allows real-time analysis of different substances, products or mixtures, without the need for traditional laboratory and sampling techniques, allowing industry to obtain results on the spot to make decisions or correct production process parameters.

The new generation Visum Palm™ brings with it an innovative design and a radical change in the way users experience NIR technology, now assisted by AI with the Visum Master™ software, so that each manufacturer can automatically create their own predictive models or calibrations according to their control and analysis needs.

Design, autonomy and robustness

The Visum Palm™ analyser offers an innovative and ergonomic design, as well as the possibility to perform analysis at any time and place without having to connect it to any external electronic device. This is possible because it incorporates an embedded touch screen and computer, which enable all the routine functionalities of the device.

The Visum Palm™ operates in the 900 to 1700 nm range, as this is the band that best combines availability of chemical information with price and technological maturity. It operates mainly in diffuse reflectance mode, for which it has specially designed and patented optics to extract as much information as possible from the sample. Specifically, it has a large illumination area (50 mm diameter) and a collection area of 10 mm. These features differentiate it from similar analysers in terms of its suitability for analysing heterogeneous samples, which is most often the case in real working conditions. In cases where heterogeneity is more evident, the device is configurable to calculate and report the average of a given number of repetitions.

The Visum Palm™ analyser is IP65 compliant, making it resistant to dust, moisture and water. It is also rugged enough to be carried and tested almost anywhere indoors or outdoors and even comes with a stand for desktop or tabletop use.

A new AI-assisted user experience

Unlike most common modelling and calibration software on the market, which requires the user to have some technical knowledge of chemometrics or entrust the task to a third party, Visum Master™ PC-based software makes NIR technology even more accessible by automating pre-processing, multivariate analysis algorithm selection and validation. This allows any user to generate models by simply inputting spectra and references (quantitative or qualitative) for routine real-time analysis to replace traditional analysis.

The new software also allows to extend and edit pre-existing models, synchronise with the portable analyser to import spectra, export models, download measurement results, automatically generate analytical method validation reports and audit reports for GMP environments, and to check the metrological performance of the device in a guided manner when needed.

For industry and GMP environments

While NIR technology has a myriad of applications in numerous industries such as plastics, food, chemical, agribusiness, wood, biofuels, to mention the most relevant but not the only ones; it is for the pharmaceutical industry and GMP environments where the new Visum Palm™ device introduces significant novelties at the level of usability and functionality. It is 21 CFR Part 11 compliant, allowing the generation and display of an automatic Audit Trail report, the record of all device activity, where comments and observations can be incorporated. It also allows the user to automatically generate the analytical method validations developed and perform metrological checks of the device when required and download the results at a later date.

“NIR technology today must be easy to use and understand, and at the same time it must give the user the freedom and autonomy to exploit it to the full and facilitate their day-to-day work. Technology must be an enabler. We will continue to take further steps in terms of automation and new functionalities because we are convinced that this is the right way forward and what the industry and the people in it need”, says Oonagh Mc Nerney, Director of IRIS Technology Solutions, S.L.

The new Visum Palm™ handheld NIR analyser is now available here, where you can also find technical information about the device, videos and contact IRIS Technology Solutions, S.L. for a demonstration or specific enquiry.

By IRIS Technology Solutions

Recycling of multilayer and composite plastics

Plastics bring value as convenient, versatile and lightweight consumer products, as well as advanced performance in high-end applications such as automobiles. However, despite their usefulness, it is clear that linear, single-use consumption of plastics is incompatible with Europe’s transition to a circular economy. This model prioritises the reuse and recycling of resources, with the aim of reducing waste and retaining as much value as possible.

In terms of plastics recycling, some progress has been made. For example, 41.5% of the plastic packaging waste generated was recycled in 2018. This is still not enough to achieve full circularity, especially in the recycling of multilayer plastics that are difficult to separate. In addition, it is essential that recycling technologies keep up with new materials entering the market

Advanced plastics recycling

The EU-funded MultiCycle project aims to develop a pilot plant for industrial recycling and treatment of multilayer plastics. This plant focuses on two important industrial segments that pose a challenge for recyclers: multilayer packaging/flexible films and fibre-reinforced thermoplastic composites of the type used in the automotive sector.

Technology selection

NIR and HSI-NIR are the techniques conventionally used for container sorting. The former is suitable for individual pieces of packaging prior to shredding and can also provide an initial assessment of suitability before moving on to the latter, which provides a mode of imaging. In the MultiCycle project, packaging materials were fed onto a conveyor in the form of flakes up to 5 cm and therefore HSI was the target technique for final implementation in the prototype incoming control system. However, point NIR spectroscopy was the target technique used for monitoring dissolved and recovered plastics during and after the CreaSolv® process, where no imaging capability is required. Complementary techniques such as LIBS and FTIR have also been preliminarily tested to detect other fractions such as AlOx or to enable the detection of black containers, which could improve the accuracy of monitoring when a full system is implemented.

Near Infrared Spectroscopy (NIRS)

NIR spectroscopy is a vibrational spectroscopic technique. In this region, absorption spectra are composed of overtones and combination bands with respect to the fundamental modes of molecules in the mid-infrared region. NIR radiation has a wavelength range of 900 to 2500 nm. The absorption bands in this region are broad, due to the high degree of band overlap. In addition, due to the selection rules of the phenomena, the signal intensity is ten to a thousand times weaker than signals in the mid-infrared region. However, this lack of intensity and the high band overlap is compensated by its high specificity. The specificity of NIR spectroscopy is based on the fact that NH, OH and CH bonds strongly absorb radiation at these wavelengths, which makes it an optimal tool for the study of organic compounds and polymers. In addition, the use of multivariate methods for the analysis of spectral data has made it possible to exploit the full potential of the technique for identification, discrimination, classification and quantification purposes.

Hyperspectral imaging system in the shortwave infrared region (HSI-SWIR)

Current technologies for the monitoring and classification of solid plastic waste in the near-infrared region have incorporated hyperspectral cameras in their configuration. They allow, instead of collecting a single spectrum, to record a hyperspectral image (HSI) of the sample (hyperspectral cube), which contains not only the spatial location of the sample, but also its chemical composition and distribution. In this regard, several publications and technological developments have been made using HSI-SWIR for the classification and identification of plastics.

A basic hyperspectral imaging system, shown in Fig.3, includes in its configuration, a sensitive sensor (CCD camera); a broadband illumination source; a spectrometer, which separates the backscattered/transmitted light into its different wavelengths and, when required, a conveyor belt for sampling. In this case, it should be noted that the conveyor belt must be synchronised with the recording speed of the CCD sensor for proper image acquisition. A hyperspectral system provides a hypercube as output. A hypercube is a set of data arranged in three dimensions, two spatial (an XY plane) and one spectral (𝜆, wavelength), as depicted below.

Measurement parameters:

The most relevant parameters for hyperspectral cube recording can be summarised as follows:

Camera frame rate (fps)
Transporter speed (m/s)
Camera-transporter distance (cm) and collection time (µs). These parameters are interrelated and must be optimised to obtain good quality recorded spectra.

The hyperspectral images were recorded with a SWIR camera operating in the range ∼900-1700 nm, at a frame rate of 214 fps, with an integration time of 350𝜇s and a transporter speed of 25m/min.

Figure 1: (Left) Sample set no. 1. Includes flexible plastic films of PE, PP, PA and PET. Single and double combinations of these polymers (i.e. polymer A/polymer B) were included. (Right) Classification image made by a PLSDA model.

Project conclusions

The HSI monitoring system has been able to provide a good approximation of the percentage of polymer content in a multilayer polymer sample. In the worst case, the most abundant polymer present in the sample is predicted, so with large batches, the final percentages would be fairly accurate. In terms of monitoring the dissolution process, only 1 polymer and 1 solvent were provided for testing in IRIS. The results obtained with Visum Palm™ were as expected, but no process models were tested over time. The dissolution control was not performed due to problems with the viscometer installed in LOEMI. For this reason, there are no further results in this section.

For the monitoring of the automotive samples, the selected technique was LIBS. The optimisation of LIBS was complicated, as it was the first time it was used. Models were run by changing different parameters to select the best conditions. The PATbox tool for LIBS did not allow data acquisition at the same speed as the LIBS software, so the models had to be modified. Finally, the models were calibrated and tested to predict the type of fibres in the black plastics PP and PA. The results obtained in the 3 batches were satisfactory, as the predictions given by the models (chemometrics and machine learning) were close to the real content. Some tests were performed to differentiate between PP and PA, but the classification rate was around 80% of good predictions. In general, mislabelling and soiling of the samples were not very useful for the development of the prediction models.

By IRIS Technology Solutions

Circular Economy: Bioplastics vs. black plastics

By 2022, a significant share of used plastics – in some countries more than two thirds – will be incinerated or sent to landfill, and only a small share will be recycled (30%). In this context, there is an urgent need to find biodegradable substitute materials for black plastics that cannot be recovered today by traditional optical and sorting techniques, while maintaining their functional properties in industrial applications.

In this context, IRIS Technology presented last July at SIMULTECH 2022, its research “Biodegradation prediction and modelling for decision support”, a mathematical AI model that allows predicting the biodegradation of natural materials of food origin that are candidates to replace carbon compounds currently used in the automotive industry, electronics, plastic bags, among others.

Bioplastics and black plastics

The term bioplastic is a complex one, encompassing materials that come from renewable sources and materials that are biodegradable. While many plastics, under certain natural or man-made conditions, are degradable, not all are recoverable. In particular, black plastics, because of their pigment or colour, escape the traditional infrared systems used in the recycling industry for their separation.

BionTop

The work being carried out by IRIS Technology together with a dozen European entities falls under the umbrella of the European BIOnTop project, which aims to develop a range of bioplastics and complementary coatings and validate their use in food and personal care packaging, determining their environmental impact and the economic viability of an extended substitution project in the industry.

Administrations and Companies participating in the project

Germany: European Bioplastics EV, Fachhochschule Albstadt-Sigmaringen
Belgium: Istrazivanjei Razvoj Centre Scientifique & Technique del’Industrie Textile Belge ASBL, Organic Waste Systems NV, Sioen Industries NV
Slovenia: BIO-Mi Drustvo S Ogranicenom Odgovornoscu za Proizvodnju
Spain: AIMPLAS, Cristobal Meseguer SA, Emsur Macdonell SA, IRIS Technology Solutions SL, Queserías Entrepinares SA, Ubesol SL
Estonia: Wearebio OU
Italy: Consorzio Interuniversitario Nazionale per la Scienza e Tecnologia dei Materiali, Enco SRL, Laboratori Archa SRL, Movimento Consumatori, Planet Bioplastics SRL, Romei SRL
Netherlands: Total Corbion PLA BV
Czech Republic: Silon SRO

By IRIS Technology Solutions

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Real-time monitoring of free lacticide during the production of PLA (polylactic acid)

Monitoring of free lacticide levels during PLA (polylactic acid) production in real-time.

Reactive extrusion - REX

Polylactic acid (PLA)

Visum NIR In-Line Probe™ as a control tool to monitor PLA synthesis by reactive extrusion

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Raman Process Analyzer: Innovation in Industrial Process Control

Innovation in industrial process control thanks to the Visum Raman In-Line™ Raman process analyzer

What is Raman spectroscopy?

Applications of Raman technology in industry

Raman Process Analyzer Visum Raman In-Line™: Innovation and precision for in-line analysis

Why choose the Raman Process Analyzer Visum Raman In-Line™?

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NIRS analysis of Brix degrees in whole apples in real time

Analysis of Brix degrees

Traditional analysis of brix degrees in apples

Advantages of NIRS technology

Brix analysis of apples with NIR spectroscopy

Conclusions: NIRS analysis of Brix degrees

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Water Activity Analysis in animal feed with Visum Palm™ portable NIR

Water Activity Analysis in animal feed with Visum Palm™ portable NIR

Water Activity Analysis in animal feed

Traditional Analysis Method

Determination of water activity with NIRS in seconds

Importance of Water Content Analysis for Food Safety

Conclusions of analysis of water activity in animal feed

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Real-time cooking degree monitoring of gummies with Visum Raman In-Line™

Real-time cooking degree monitoring of gummies with Visum Raman In-Line™

Level of starch cooking: the gelatinisation process

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A partnership for the future of the industry

Developing a real-time analytical method

Conclusions

Key features of the Visum Raman In-Line™ Process Analyser

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Plastic identification, verification and classification using Visum Palm™

Plastic identification, verification and classification using Visum Palm™

Extend and develop your own library with Visum Master™

Plastic identification

Polymer Verification

Plastic classification

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IRIS Technology Solutions at Alimentaria FoodTech 2023

IRIS Technology Solutions at Alimentaria FoodTech 2023

Visum® Solutions

Shealthy Project

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New Visum Palm™ AI-assisted handheld NIR analyser

New Visum Palm™ AI-assisted handheld NIR analyser

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Recycling of multilayer and composite plastics

Advanced plastics recycling

Technology selection

Near Infrared Spectroscopy (NIRS)

Hyperspectral imaging system in the shortwave infrared region (HSI-SWIR)

Measurement parameters:

Project conclusions

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Circular Economy: Bioplastics vs. black plastics

Circular Economy: Bioplastics vs. black plastics

Bioplastics and black plastics

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Administrations and Companies participating in the project

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